# P2P synthesis from BMK glycidate ethers



## G.Patton

*Introduction*​Hydrolysis of BMK glycidate ethers is represented in this topic. The procedure is the same for ethyl (Et) [*cas 41232-97-7*] and methyl (Me) [*cas 80532-66-7*] esters of glycidic acid. In case of sodium (Na) salt of this acid [*cas 5449-12-7*], you can skip first stage of NaOH addition and start from acid hydrolysis. In addition, purification method of obtained P2P is described. This procedure have to be committed to get pure Phenylacetone (P2P) for further syntheses of methamphetamine or amphetamine.

Suppliers of BMK glycidate ethers can be found in *BB Listing*.

*Difficulty rating:* 2/10


​
*Equipment and **glassware:*

1000 mL Round bottom flask;
Reflux condenser;
Retort stand and clamp for securing apparatus;
pH indicator paper;
Vacuum source (optional);
Rotovap machine (optional);
Glass rod and spatula;
100 mL x2; 250 mL x2; 500 mL x2 Beakers;
Magnetic or top stirrer with a heating plate;
Water bath;
Funel;
1000 mL Separatory funnel;
Vacuum distillation setup (optional);

*Reagents:*​
100 g BMK glycidate ethers (cas 80532-66-7; cas 41232-97-7; cas 5449-12-7);
~20 g NaOH or KOH;
~80 ml HCl (35%) or 100 ml H2SO4 (45%);
~600 mL DCM or Petroleum Ether;
~100 g MgSO4 or Na2SO4;
~500-600 mL Distilled water;
~ 50 g NaCl (optional);


​*Hydrolysis of BMK glycidates*​*1.* NaOH (or KOH) 20g is dissolved in 250-300 ml distilled water with stirring. The reaction mixture (Rm) have to be cooled to room temperature. BMK glycidate 100 g (methyl or ethyl ester) is added and dissolved completely. Part of BMK is hydrolyzed during this procedure and floated as an oil in the surface of Rm. Rm is stired for 1 h at 75-80 °C with a reflux condenser.
*2.* Then, 200 ml HCl (35%) or 240 ml H2SO4 (45%) are added in small portions to Rm and heated to 80-90 °C and stired for 3 h. Rm have to be cooled to room temperature, the precipitate is filtered.
*3.* The reaction solution is extracted with DCM or petroleum ether 3 x 100 ml. Extract is washed with brine to neutral pH 7 several times. Extract is dried with MgSO4 (or Na2SO4) (optional) and filtered from solids.
*4.* An organic solvent (DCM or petroleum ether) is distilled off to give 65 ml of P2P.
​*P2P purification*​*1.* The resulting phenylacetone (P2P) is transferred to a round bottom flask with distilled water 1:1 (w/w) and distilled with steam under vacuum.
*2.* Purified P2P from receiver flask is extracted from water mixture with DCM (or petroleuum ether) 3 x 100 mL. Extract is dried with MgSO4 (or Na2SO4).
*3.* The resulting solution is filtered from the solids (drying agent) and then an organic solvent is distilled off.

Phenylacetone can be stored long time in a sealed vessel in a freezer. It is recommended to distill it before further syntheses of methamphetamine or amphetamine. Avoid direct sunlight onto phenylacetone and exposure to high temperatures.​


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## T0R

this is the preparation of P2P Phenylacetone CAS 103-79-7 made use of BMK Glycidic Acid ( sodium salt ) CAS 5449-12-7 with main ingredient sulfonic acid strength is 75% CAS 7664-38-2
-------------------------------------------------- ------------------------------
we are going to prepare 1 kg of BMK
take a 5 liter double neck flask
add 500ml boiling water . start with the mixer.
now slowly add 1kg of BMK salt. then add 1 liter of sulfonic acid. now connect the reflux and heat the contents of the flask to max temperature. plus minus 130°c. use a powerful mixer
Let it boil in reflux for 4 hours.
take the top layer and pour it into a measuring cup.
let the bottom layer cool and save for next time. ( we have no chemical waste for this preparation method )

now boil 1 liter of water and add it to the measuring cup. use a hand mixer to mix everything.
After mixing for a few minutes, let the measuring cup cool to room temperature.
remove the top white layer (this is water and waste that we don't need)
the bottom layer is P2P purified and ready to use.

ps: in this preparation we don't have to worry about water remaining in our P2P because water weighs less than P2P

ps2: if you keep these ratios, the P2P will have a ph value of 4 .
if you use more sulfonic acid the ph value will drop to 1. Therefore it is not necessary to use too much sulfonic acid.


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## G.Patton

Saul said:


> edit // VERY slowly in a liter of 80°c phosphoric acid (NO WATER)



SaulDo you use H3PO4 cons or diluted solution? Thank you for your feedback.


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## T0R

No, this I did in my second attempt I had an orange very light color. Then 

PS : my re use bottom layer 1liter weight 1,675 kg color is (pisang ambon )


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## KokosDreams

Saul said:


> I use a very powerful mixer.



SaulHey man,

can you send me the mixer/stirrer you are using via PM?
I am about to order mine and don't want to buy a shitty one.

Any help is highly appreciated.

Thanks

Koko


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## T0R

KokosDreams said:


> Hey man,
> 
> can you send me the mixer/stirrer you are using via PM?
> I am about to order mine and don't want to buy a shitty one.
> 
> Any help is highly appreciated.
> 
> Thanks
> 
> Koko



KokosDreams
yes no problem


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## T0R

for privacy reasons Iam not gonna give you the link off my mixer. 
but with this info you have enouch . 
it takes me 3 different orders and not at the same time .

There are 3 different orders for 1 mixer 

1/ the mixer 110watt AliExpress with stand and clamps
2/ 8 mm drilled head , you can use rod diameter from 1 till 10 mm ( original you only can use diameter 6 mm ) 
3/ rod minimum 450 mm diameter 10 not so easy to find a good one )


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## KokosDreams

Saul said:


> yes no problem



SaulAmaying


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## KokosDreams

Saul said:


> for privacy reasons Iam not gonna give you the link off my mixer.
> but with this info you have enouch .
> it takes me 3 different orders and not at the same time .
> 
> There are 3 different orders for 1 mixer
> 
> 1/ the mixer 110watt AliExpress with stand and clamps
> 2/ 8 mm drilled head , you can use rod diameter from 1 till 10 mm ( original you only can use diameter 6 mm )
> 3/ rod minimum 450 mm diameter 10 not so easy to find a good one )



SaulNo worries man!

That was already a good help.

I was looking at one with 100W and 3.000rpm - do you think the 10W difference will be too signicigant?


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## T0R

no its fine !


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## KokosDreams

Saul said:


> no its fine !



SaulThanks man!


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## G.Patton

Saul said:


> No, this I did in my second attempt I had an orange very light color. Then
> 
> PS : my re use bottom layer 1liter weight 1,675 kg color is (pisang ambon )



SaulI asked about acid solution.


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## jasper12

does hci 30% works the same like hci 37 in the whole process?


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## G.Patton

jasper12 said:


> does hci 30% works the same like hci 37 in the whole process?



jasper12Yes, if you use proportionately more acid.


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## T0R

G.Patton said:


> Do you use H3PO4 cons or diluted solution? Thank you for your feedback.



G.Patton
I use cas7664-38-2 
75%


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## Jesse_Pinkman_

I buyed this one...but did not use it yet.
It has a heating and stirring function, but i dont know how much rpm, just 350W.
Any experiences?


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## KokosDreams

350W might be good depending on the volume you want to heat/stir.

Heating Mantles are a great addition for any lab!


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## Jesse_Pinkman_

This one is for 1000ml flask, not very much but was the only which available. There are 2000ml on the market but not at that time i buyed. So i will have to do a lot of small steps.
Or i use other kind of heat/stirring products at the same time...however, i will start with small scale to test my knowlegde. I had no practice till now, only theory by reading articles/posts and watching videos. My motherlanguage is not english, so i had to translate a lot of words i did not knew before, what makes it difficult sometime to understand every single word. But i will keep on reading and learning.
This is some of my equipment


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## KokosDreams

Jesse_Pinkman_ said:


> This one is for 1000ml flask, not very much but was the only which available. There are 2000ml on the market but not at that time i buyed. So i will have to do a lot of small steps.
> Or i use other kind of heat/stirring products at the same time...however, i will start with small scale to test my knowlegde. I had no practice till now, only theory by reading articles/posts and watching videos. My motherlanguage is not english, so i had to translate a lot of words i did not knew before, what makes it difficult sometime to understand every single word. But i will keep on reading and learning.
> This is some of my equipment



Jesse_Pinkman_Exciting  Good luck!


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## Jesse_Pinkman_

KokosDreams said:


> Exciting  Good luck!



KokosDreamsThx Buddy


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## merlin

G.Patton said:


> *Introduction*​Hydrolysis of BMK glycidate ethers is represented in this topic. The procedure is the same for ethyl (Et) [*cas 41232-97-7*] and methyl (Me) [*cas 80532-66-7*] esters of glycidic acid. In case of sodium (Na) salt of this acid [*cas 5449-12-7*], you can skip first stage of NaOH addition and start from acid hydrolysis. In addition, purification method of obtained P2P is described. This procedure have to be committed to get pure Phenylacetone (P2P) for further syntheses of methamphetamine or amphetamine.
> 
> Suppliers of BMK glycidate ethers can be found in *BB Listing*.
> 
> *Difficulty rating:* 2/10View attachment 6617​
> *Equipment and **glassware:*
> 
> 1000 mL Round bottom flask;
> Reflux condenser;
> Retort stand and clamp for securing apparatus;
> pH indicator paper;
> Vacuum source (optional);
> Rotovap machine (optional);
> Glass rod and spatula;
> 100 mL x2; 250 mL x2; 500 mL x2 Beakers;
> Magnetic or top stirrer with a heating plate;
> Water bath;
> Funel;
> 1000 mL Separatory funnel;
> Vacuum distillation setup (optional);
> 
> *Reagents:*​
> 100 g BMK glycidate ethers (cas 80532-66-7; cas 41232-97-7; cas 5449-12-7);
> ~20 g NaOH or KOH;
> ~80 ml HCl (35%) or 100 ml H2SO4 (45%);
> ~600 mL DCM or Petroleum Ether;
> ~100 g MgSO4 or Na2SO4;
> ~500-600 mL Distilled water;
> ~ 50 g NaCl (optional);
> View attachment 6616​*Hydrolysis of BMK glycidates*​*1.* NaOH (or KOH) 20g is dissolved in 250-300 ml distilled water with stirring. The reaction mixture (Rm) have to be cooled to room temperature. BMK glycidate 100 g (methyl or ethyl ester) is added and dissolved completely. Part of BMK is hydrolyzed during this procedure and floated as an oil in the surface of Rm. Rm is stired for 1 h at 75-80 °C with a reflux condenser.
> *2.* Then, 200 ml HCl (35%) or 240 ml H2SO4 (45%) are added in small portions to Rm and heated to 80-90 °C and stired for 3 h. Rm have to be cooled to room temperature, the precipitate is filtered.
> *3.* The reaction solution is extracted with DCM or petroleum ether 3 x 100 ml. Extract is washed with brine to neutral pH 7 several times. Extract is dried with MgSO4 (or Na2SO4) (optional) and filtered from solids.
> *4.* An organic solvent (DCM or petroleum ether) is distilled off to give 65 ml of P2P.​*P2P purification*​*1.* The resulting phenylacetone (P2P) is transferred to a round bottom flask with distilled water 1:1 (w/w) and distilled with steam under vacuum.
> *2.* Purified P2P from receiver flask is extracted from water mixture with DCM (or petroleuum ether) 3 x 100 mL. Extract is dried with MgSO4 (or Na2SO4).
> *3.* The resulting solution is filtered from the solids (drying agent) and then an organic solvent is distilled off.
> 
> Phenylacetone can be stored long time in a sealed vessel in a freezer. It is recommended to distill it before further syntheses of methamphetamine or amphetamine. Avoid direct sunlight onto phenylacetone and exposure to high temperature​



G.Patton
It would be good if we had one like this pmk to mdma


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## Jesse_Pinkman_

merlin said:


> It would be good if we had one like this pmk to mdma



merlinHere: 


A Photo Essay on the Nitromethane Al/Hg


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## G.Patton

merlin said:


> It would be good if we had one like this pmk to mdma



merlinHello, can you ask more clearly please? Do you want to convert PMK glycidate to MDP2P and than to MDMA? There is* method *on our forum how to get MDP2P. MDP2P -> MDMA. Look around Amphetamines forum section. 
Synthesis of MDMA from piperonylmethylketone (PMK) with formamide and LAH
Synthesis of MDMA via Pt/H2 (small scale)



Jesse_Pinkman_ said:


> Here:
> 
> 
> A Photo Essay on the Nitromethane Al/Hg


Hello, you can advice our forum topics with better explanation as well. I would be very appreciated. There is method with pictures Complete MDMA synthesis from sassafras oil. There are photos of stages from MDP2P to MDMA and detailed explanation.


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## Mr.Blanks00

Sir, I want to ask, how do we test that the reagents we make are p2p correct.


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## G.Patton

Yusuf said:


> Sir, I want to ask, how do we test that the reagents we make are p2p correct.



YusufFirst of all, you can cheek general appearance and than measure boiling point.


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## heliosyang

Is the starting material [cas 41232-97-7] or [cas 80532-66-7]?


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## G.Patton

heliosyang said:


> Is the starting material [cas 41232-97-7] or [cas 80532-66-7]?



heliosyangHello, you can use both of them as precursor.


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## diogenes

Can anyone advice on which precursor is best to buy I mean safest to ship to Europe? Is any of the BMK powders legal - where can this be checked? I`m a bit confused as there are quite a few versions available.


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## KokosDreams

diogenes said:


> Can anyone advice on which precursor is best to buy I mean safest to ship to Europe? Is any of the BMK powders legal - where can this be checked? I`m a bit confused as there are quite a few versions available.



diogenes
P2NP is legal
P2P is restricted
BMK Glycidate 5449 is still quite new and as far as I know not restricted, altho it is common knowledge what glycidates are used for, especially bmk glycidates.

My guess would be that P2NP is the safest bet


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## T0R

KokosDreams said:


> P2NP is legal
> P2P is restricted
> BMK Glycidate 5449 is still quite new and as far as I know not restricted, altho it is common knowledge what glycidates are used for, especially bmk glycidates.
> 
> My guess would be that P2NP is the safest bet



KokosDreams
1-Phenyl-2-nitropropene, or simply phenyl-2-nitropropene, or P2NP, as it is commonly ... amphetamine class, and are listed as drug precursors in many countries








Phenyl-2-nitropropene - Wikipedia







en.wikipedia.org





Bmk salt cas 5449-12-7 is still verry new in de scene it is worldwide allowd and till today not listed in no country.

also prices off P2NP go with the wind I mean not stable prices . the bmk salt is sent from europe with secure shipping line
it cost something like 100€ / kg


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## KokosDreams

Saul said:


> 1-Phenyl-2-nitropropene, or simply phenyl-2-nitropropene, or P2NP, as it is commonly ... amphetamine class, and are listed as drug precursors in many countries
> 
> 
> 
> 
> 
> 
> 
> 
> Phenyl-2-nitropropene - Wikipedia
> 
> 
> 
> 
> 
> 
> 
> en.wikipedia.org
> 
> 
> 
> 
> 
> Bmk salt cas 5449-12-7 is still verry new in de scene it is worldwide allowd and till today not listed in no country.
> 
> also prices off P2NP go with the wind I mean not stable prices . the bmk salt is sent from europe with secure shipping line
> it cost something like 100€ / kg



Saul
P2NP is not restricted so far in most of the countries.


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## T0R

KokosDreams said:


> P2NP is not restricted so far in most of the countries.



KokosDreams
I copy paste from pedia


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## KokosDreams

Saul said:


> I copy paste from pedia



Saul
Yeah the Wikipedia article is actually a little wrong. There are much more usecases for P2NP and it's not restricted


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## caesare.robot

SWIM started with [*cas 5449-12-7*] after 4h of heating got aqueous layer on top and oily bottom... what did wrong? too much acid?


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## caesare.robot

caesare.robot said:


> SWIM started with [*cas 5449-12-7*] after 4h of heating got aqueous layer on top and oily bottom... what did wrong? too much acid?



caesare.robotfurther attempts with *cas 5449-12-7* and step 1 of described method gave proper and stable results!


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## ChingShih

caesare.robot said:


> SWIM started with [*cas 5449-12-7*] after 4h of heating got aqueous layer on top and oily bottom... what did wrong? too much acid?



caesare.robot
Please post some pictures, there should be no problem i think


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## T0R

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/p2p-synthesis-from-bmk-glycidate-ethers.4307/post-13418


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## caesare.robot

as far SWIM understands the P2P oily layer should float after reflux and heating? (temperature was constant 90°C. PH1.)


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## Sweswe

caesare.robot said:


> as far SWIM understands the P2P oily layer should float after reflux and heating? (temperature was constant 90°C. PH1.)



caesare.robotYou have some pictures?


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## G.Patton

caesare.robot said:


> as far SWIM understands the P2P oily layer should float after reflux and heating? (temperature was constant 90°C. PH1.)



caesare.robotPhenylacetone (P2P) has Density: 1.0057 g/cm3; Hence - your layer heavier than water. It means that it have to be on a bottom. Vice versa, if your water layer is heavier by reason of dissolved salts, p2p layer will be on a top. What is a problem to check boiling point?


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## h20

caesare.robot said:


> as far SWIM understands the P2P oily layer should float after reflux and heating? (temperature was constant 90°C. PH1.)



caesare.robot


G.Patton said:


> Phenylacetone (P2P) has Density: 1.0057 g/cm3; Hence - your layer heavier than water. It means that it have to be on a bottom. Vice versa, if your water layer is heavier by reason of dissolved salts, p2p layer will be on a top. What is a problem to check boiling point?



This is a very interesting question.
If we cook BMK salts, then the top layer is the p2p
if we now pour this top layer into a measuring cup, and we add warm water. Then the water is the top layer.


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## caesare.robot

SWIM started with [*cas 5449-12-7*] after 4h of heating got aqueous layer on top and oily bottom... what did wrong? too much acid?


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## caesare.robot

caesare.robot said:


> SWIM started with [*cas 5449-12-7*] after 4h of heating got aqueous layer on top and oily bottom... what did wrong? too much acid?



caesare.robotfurther attempts with *cas 5449-12-7* and step 1 of described method gave proper and stable results!


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## Evilcarrot2

Can cas 77-83-8 be used?


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## G.Patton

Evilcarrot2 said:


> Can cas 77-83-8 be used?



Evilcarrot2no, you won't get P2P


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## Evilcarrot2

G.Patton said:


> no, you won't get P2P



G.PattonAs always thank you


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## ossi

G.Patton said:


> *Introduction*​Hydrolysis of BMK glycidate ethers is represented in this topic. The procedure is the same for ethyl (Et) [*cas 41232-97-7*] and methyl (Me) [*cas 80532-66-7*] esters of glycidic acid. In case of sodium (Na) salt of this acid [*cas 5449-12-7*], you can skip first stage of NaOH addition and start from acid hydrolysis. In addition, purification method of obtained P2P is described. This procedure have to be committed to get pure Phenylacetone (P2P) for further syntheses of methamphetamine or amphetamine.
> 
> Suppliers of BMK glycidate ethers can be found in *BB Listing*.
> 
> *Difficulty rating:* 2/10View attachment 6617​
> *Equipment and **glassware:*
> 
> 1000 mL Round bottom flask;
> Reflux condenser;
> Retort stand and clamp for securing apparatus;
> pH indicator paper;
> Vacuum source (optional);
> Rotovap machine (optional);
> Glass rod and spatula;
> 100 mL x2; 250 mL x2; 500 mL x2 Beakers;
> Magnet-  oder Aufsatzrührer mit Heizplatte;
> Wasserbad;
> Trichter;
> 1000 ml Scheidetrichter;
> Einrichtung zur Vakuumdestillation (optional);
> 
> *Reagenzien:*​
> 100 g BMK-Glycidatether (cas 80532-66-7; cas 41232-97-7; cas 5449-12-7);
> ~20 g NaOH oder KOH;
> ~80 ml HCl (35 %) oder 100 ml H2SO4 (45 %);
> ~600 ml DCM oder Petrolether;
> ~100 g MgSO4 oder Na2SO4;
> ~500–600 ml destilliertes Wasser;
> ~ 50 g NaCl (optional);
> View attachment 6616​*Hydrolyse von BMK-Glycidaten*​*1.* NaOH (oder KOH) 20 g werden in 250-300 ml destilliertem Wasser unter Rühren gelöst. Das Reaktionsgemisch (Rm) muss auf Raumtemperatur gekühlt werden. 100 g BMK-Glycidat (Methyl- oder Ethylester) werden zugegeben und vollständig gelöst. Ein Teil von BMK wird dabei hydrolysiert und schwimmt als Öl an der Oberfläche von Rm. Rm wird 1 h bei 75-80 °C mit einem Rückflusskühler gerührt .
> *2.* Dann werden 200 ml HCl (35 %) oder 240 ml H2SO4 (45 %) in kleinen Portionen zu Rm gegeben und auf 80-90 °C erhitzt und 3 h gerührt. Rm müssen auf Raumtemperatur abgekühlt werden, der Niederschlag wird filtriert.
> *3.* Die Reaktionslösung wird mit DCM oder Petrolether 3 x 100 ml extrahiert . Der Extrakt wird mehrmals mit Salzlösung auf einen neutralen pH-Wert von 7 gewaschen . Der Extrakt wird mit MgSO4 (oder Na2SO4) (optional) getrocknet und von Feststoffen filtriert.
> *4.* Ein organisches Lösungsmittel (DCM oder Petrolether) wird abdestilliert, um 65 ml P2P zu ergeben.​*P2P-Reinigung*​*1.* Das entstandene Phenylaceton (P2P) wird in einen Rundkolben mit destilliertem Wasser 1:1 (w/w) überführt und mit Wasserdampf unter Vakuum destilliert .
> *2.* Gereinigtes P2P aus dem Auffangkolben wird aus einer Wassermischung mit DCM (oder Petrolether) 3 x 100 ml extrahiert. Der Extrakt wird mit MgSO4 (oder Na2SO4) getrocknet.
> *3.* Die resultierende Lösung wird von den Feststoffen (Trockenmittel) filtriert und dann wird ein organisches Lösungsmittel abdestilliert.
> 
> Phenylaceton kann lange Zeit in einem verschlossenen Gefäß in einem Gefrierschrank gelagert werden. Es wird empfohlen, es vor weiteren Synthesen von Methamphetamin oder Amphetamin zu destillieren . Direkte Sonneneinstrahlung auf Phenylaceton und hohe Temperaturen vermeiden.​



G.Pattonmaybe this works with benzylcyanid?


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## G.Patton

ossi said:


> maybe this works with benzylcyanid?



ossino


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## Costa

G.Patton said:


> *Introduction*​Hydrolysis of BMK glycidate ethers is represented in this topic. The procedure is the same for ethyl (Et) [*cas 41232-97-7*] and methyl (Me) [*cas 80532-66-7*] esters of glycidic acid. In case of sodium (Na) salt of this acid [*cas 5449-12-7*], you can skip first stage of NaOH addition and start from acid hydrolysis. In addition, purification method of obtained P2P is described. This procedure have to be committed to get pure Phenylacetone (P2P) for further syntheses of methamphetamine or amphetamine.
> 
> Suppliers of BMK glycidate ethers can be found in *BB Listing*.
> 
> *Difficulty rating:* 2/10View attachment 6617​
> *Equipment and **glassware:*
> 
> 1000 mL Round bottom flask;
> Reflux condenser;
> Retort stand and clamp for securing apparatus;
> pH indicator paper;
> Vacuum source (optional);
> Rotovap machine (optional);
> Glass rod and spatula;
> 100 mL x2; 250 mL x2; 500 mL x2 Beakers;
> Magnetic or top stirrer with a heating plate;
> Water bath;
> Funel;
> 1000 mL Separatory funnel;
> Vacuum distillation setup (optional);
> 
> *Reagents:*​
> 100 g BMK glycidate ethers (cas 80532-66-7; cas 41232-97-7; cas 5449-12-7);
> ~20 g NaOH or KOH;
> ~80 ml HCl (35%) or 100 ml H2SO4 (45%);
> ~600 mL DCM or Petroleum Ether;
> ~100 g MgSO4 or Na2SO4;
> ~500-600 mL Distilled water;
> ~ 50 g NaCl (optional);
> View attachment 6616​*Hydrolysis of BMK glycidates*​*1.* NaOH (or KOH) 20g is dissolved in 250-300 ml distilled water with stirring. The reaction mixture (Rm) have to be cooled to room temperature. BMK glycidate 100 g (methyl or ethyl ester) is added and dissolved completely. Part of BMK is hydrolyzed during this procedure and floated as an oil in the surface of Rm. Rm is stired for 1 h at 75-80 °C with a reflux condenser.
> *2.* Then, 200 ml HCl (35%) or 240 ml H2SO4 (45%) are added in small portions to Rm and heated to 80-90 °C and stired for 3 h. Rm have to be cooled to room temperature, the precipitate is filtered.
> *3.* The reaction solution is extracted with DCM or petroleum ether 3 x 100 ml. Extract is washed with brine to neutral pH 7 several times. Extract is dried with MgSO4 (or Na2SO4) (optional) and filtered from solids.
> *4.* An organic solvent (DCM or petroleum ether) is distilled off to give 65 ml of P2P.​*P2P purification*​*1.* The resulting phenylacetone (P2P) is transferred to a round bottom flask with distilled water 1:1 (w/w) and distilled with steam under vacuum.
> *2.* Purified P2P from receiver flask is extracted from water mixture with DCM (or petroleuum ether) 3 x 100 mL. Extract is dried with MgSO4 (or Na2SO4).
> *3.* The resulting solution is filtered from the solids (drying agent) and then an organic solvent is distilled off.
> 
> Phenylacetone can be stored long time in a sealed vessel in a freezer. It is recommended to distill it before further syntheses of methamphetamine or amphetamine. Avoid direct sunlight onto phenylacetone and exposure to high temperatures.​



G.PattonHi, could you answer some doubts?

3.- What is the pH in this stage after wahsing with DCM? The wash with brine is mandatory? If yes, what is the concentration of NaCl solution? 
4.- This is simple distilation at DCM boling point (around 40ºC) rigth? 

P2P Purification is worthy in yield terms to reach amphetamine? If yes, do you know how much does it increase?

1.- What is the point of mixing with water (65 ml), and distill again to separete from water? or could we have some unwanted components?
What is the pressure and the temperature in this stage for the vacuum distilation? 
Is possible simple distilation without vacuum? Around water boiling point (100ºC)


​


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## G.Patton

Costa said:


> Hi, could you answer some doubts?
> 
> 3.- What is the pH in this stage after wahsing with DCM? The wash with brine is mandatory? If yes, what is the concentration of NaCl solution?
> 4.- This is simple distilation at DCM boling point (around 40ºC) rigth?
> 
> P2P Purification is worthy in yield terms to reach amphetamine? If yes, do you know how much does it increase?
> 
> 1.- What is the point of mixing with water (65 ml), and distill again to separete from water? or could we have some unwanted components?
> What is the pressure and the temperature in this stage for the vacuum distilation?
> Is possible simple distilation without vacuum? Around water boiling point (100ºC)
> 
> 
> ​



Costa>3


> Extract is washed with brine to neutral pH 7 several times.


25% NaCl aq is okay and yes. It is necessary.
>4
Yes, you are right. You can use rotovap.
>P2P Purification is worthy in yield terms to reach amphetamine? If yes, do you know how much does it increase?
yes, it is necessary. I can't say for sure. The difference can vary greatly.
>1.- What is the point of mixing with water (65 ml), and distill again to separete from water?
read about steam distillation in Lab FAQ section
>What is the pressure and the temperature in this stage for the vacuum distilation? 
Is possible simple distilation without vacuum? Around water boiling point (100ºC)

Depends on vacuum, I can't answer you. I think it is impossible, you'll spoil your p2p with height temperature (probably).


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## Costa

G.Patton said:


> >3
> 
> 25% NaCl aq is okay and yes. It is necessary.
> >4
> Yes, you are right. You can use rotovap.
> >P2P Purification is worthy in yield terms to reach amphetamine? If yes, do you know how much does it increase?
> yes, it is necessary. I can't say for sure. The difference can vary greatly.
> >1.- What is the point of mixing with water (65 ml), and distill again to separete from water?
> read about steam distillation in Lab FAQ section
> >What is the pressure and the temperature in this stage for the vacuum distilation?
> Is possible simple distilation without vacuum? Around water boiling point (100ºC)
> 
> Depends on vacuum, I can't answer you. I think it is impossible, you'll spoil your p2p with height temperature (probably).



G.PattonTanks so much for your quick reply!


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## Costa

G.Patton said:


> >3
> 
> 25% NaCl aq is okay and yes. It is necessary.
> >4
> Yes, you are right. You can use rotovap.
> >P2P Purification is worthy in yield terms to reach amphetamine? If yes, do you know how much does it increase?
> yes, it is necessary. I can't say for sure. The difference can vary greatly.
> >1.- What is the point of mixing with water (65 ml), and distill again to separete from water?
> read about steam distillation in Lab FAQ section
> >What is the pressure and the temperature in this stage for the vacuum distilation?
> Is possible simple distilation without vacuum? Around water boiling point (100ºC)
> 
> Depends on vacuum, I can't answer you. I think it is impossible, you'll spoil your p2p with height temperature (probably).



G.PattonHi!
I made this process, and after this step:
*"2.*_ Then, 200 ml HCl (35%) or 240 ml H2SO4 (45%) are added in small portions to Rm and heated to 80-90 °C and stired for 3 h. Rm have to be cooled to room temperature, the precipitate is filtered."_
This is what I have obtained (see the picture below). Is this the expected aspect of the reaction? and my question is: is this top layer already P2P? should I put aside this layer (and keep it) and add DCM to the rest (bottom layer) in order to extract the remaining P2P from there?

Many thanks in advance!


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## G.Patton

Costa said:


> Hi!
> I made this process, and after this step:
> *"2.*_ Then, 200 ml HCl (35%) or 240 ml H2SO4 (45%) are added in small portions to Rm and heated to 80-90 °C and stired for 3 h. Rm have to be cooled to room temperature, the precipitate is filtered."_
> This is what I have obtained (see the picture below). Is this the expected aspect of the reaction? and my question is: is this top layer already P2P? should I put aside this layer (and keep it) and add DCM to the rest (bottom layer) in order to extract the remaining P2P from there?
> 
> Many thanks in advance!
> 
> 
> View attachment 8635



CostaHello, yes, it is P2P oil. You have to separate layers and then extract water (bottom) layer by DCM. Next, combine p2p oil with DCM extracts and follow instructions (wash with brine and so on).


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## Costa

G.Patton said:


> Hello, yes, it is P2P oil. You have to separate layers and then extract water (bottom) layer by DCM. Next, combine p2p oil with DCM extracts and follow instructions (wash with brine and so on).



G.PattonIs the washing of the extract (P2P oil) with brine made the same way as the washing with DCM? I mean, when adding brine to the p2p will I get two layers? In that case which one do I have to keep?


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## G.Patton

Costa said:


> Is the washing of the extract (P2P oil) with brine made the same way as the washing with DCM? I mean, when adding brine to the p2p will I get two layers? In that case which one do I have to keep?



CostaYes, pour brine solution into separatory funnel with DCM and P2P, shake it couple minutes and decant. You need organic layer. Check pH of brine after washing. It has to be around 7 pH.


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## Costa

G.Patton said:


> Yes, pour brine solution into separatory funnel with DCM and P2P, shake it couple minutes and decant. You need organic layer. Check pH of brine after washing. It has to be around 7 pH.



G.PattonHi, I followed the procedure step by step as mentioned in the instructions and it didn't work. I made several extractions of the "water" (bottom layer) using DCM and once I combined them (pouring over the P2P layer), there was some kind of reaction because lot of solids appeared. Anyway, I continued with the procedure, just in case; so I add the brine (NaCl + water) and it was even worst... 
In your last message you told I should add DMC and brine at the same time, so today I will try following this method. 

You told I have to check the pH of the brine; what is "brine" refers to? is it the layer with NaCl (the remaining layer once I separate the oily layer with P2P)? the addition of the NaCl is just to rise the pH? why is NaCl used instead if NaOH for this objective?


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## G.Patton

Costa said:


> Hi, I followed the procedure step by step as mentioned in the instructions and it didn't work. I made several extractions of the "water" (bottom layer) using DCM and once I combined them (pouring over the P2P layer), there was some kind of reaction because lot of solids appeared. Anyway, I continued with the procedure, just in case; so I add the brine (NaCl + water) and it was even worst...
> In your last message you told I should add DMC and brine at the same time, so today I will try following this method.
> 
> You told I have to check the pH of the brine; what is "brine" refers to? is it the layer with NaCl (the remaining layer once I separate the oily layer with P2P)? the addition of the NaCl is just to rise the pH? why is NaCl used instead if NaOH for this objective?



CostaHi.


> >>>there was some kind of reaction because lot of solids appeared.


I have no idea what is it, have you checked your precursor? What are you use for this synthesis?



> >>>In your last message you told I should add DMC and brine at the same time


I wrote that you have to add them in one separatory funnel, there is no difference of addition sequence.



> >>>You told I have to check the pH of the brine; what is "brine" refers to? is it the layer with NaCl (the remaining layer once I separate the oily layer with P2P)? the addition of the NaCl is just to rise the pH? why is NaCl used instead if NaOH for this objective?


You can use distilled water for washing of your extract. Brine (NaCl aq solution) is used in order to rinse acid trace from your P2P extract. It's easy, cheap and safe. Also, it is more convenient to separate layers with brine. You have to wash the organic extract by brine until neutral pH 7.


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## Costa

G.Patton said:


> Hi.
> 
> I have no idea what is it, have you checked your precursor? What are you use for this synthesis?
> 
> 
> I wrote that you have to add them in one separatory funnel, there is no difference of addition sequence.
> 
> 
> You can use distilled water for washing of your extract. Brine (NaCl aq solution) is used in order to rinse acid trace from your P2P extract. It's easy, cheap and safe. Also, it is more convenient to separate layers with brine. You have to wash the organic extract by brine until neutral pH 7.



G.Pattongreat, thanks! I will make the extraction combining DCM and brine. Just one question, I have to make 3 extractions with 100ml DCM + brine; but, how much brine on each extraction? it doesn't matter?


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## G.Patton

Costa said:


> great, thanks! I will make the extraction combining DCM and brine. Just one question, I have to make 3 extractions with 100ml DCM + brine; but, how much brine on each extraction? it doesn't matter?



CostaYou have to *carry out extraction by DCM* and *then **wash your DCM extract with brine*. It is important. Read manual carefully and try to understand the sense of each step. In opposite case you will extract water by brine.


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## Costa

_I have no idea what is it, have you checked your precursor? What are you use for this synthesis?_

*i used: cas 5449-12-7. *I took off the P2P layer and with the rest, I made the extractions with DCM. Each extraction (the oily layer obtained when adding DCM), I combined them with the P2P. It was then when the precipitate appeared. 

Today I will not combine the P2P with the extractions, just in case... I will made the extractions with DCM and each extract, I will wash them with brine, as you told. Lets see what happens.

thanks


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## G.Patton

Costa said:


> _I have no idea what is it, have you checked your precursor? What are you use for this synthesis?_
> 
> *i used: cas 5449-12-7. *I took off the P2P layer and with the rest, I made the extractions with DCM. Each extraction (the oily layer obtained when adding DCM), I combined them with the P2P. It was then when the precipitate appeared.
> 
> Today I will not combine the P2P with the extractions, just in case... I will made the extractions with DCM and each extract, I will wash them with brine, as you told. Lets see what happens.
> 
> thanks



Costa>>>the oily layer obtained when adding DCM
not oily, you'll get DCM with dissolved P2P there.


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## Costa

Hi, as said, I repeated the process following the instructions of the document (and your comments) step by step. I got exactly the same product on this step:

 I took the oily layer (top layer, which has P2P) and once it cooled down after 10 minutes it has this aspect:

.

Then I added DCM over the other layer (the "water") in order to make the first extraction, however, this was the aspect of the mixture:


 

 

as you can see, there was some kind of white precipitate on the bottom, there were not two layers, just the white solids and the rest.
What did I do wrong? The document is not very clear... 
Many thanks in advance and sorry for that many questions, but this process it is being a headache...


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## G.Patton

Costa said:


> Hi, as said, I repeated the process following the instructions of the document (and your comments) step by step. I got exactly the same product on this step:View attachment 8916 I took the oily layer (top layer, which has P2P) and once it cooled down after 10 minutes it has this aspect:View attachment 8917.
> 
> Then I added DCM over the other layer (the "water") in order to make the first extraction, however, this was the aspect of the mixture:
> View attachment 8918 View attachment 8919 View attachment 8920as you can see, there was some kind of white precipitate on the bottom, there were not two layers, just the white solids and the rest.
> What did I do wrong? The document is not very clear...
> Many thanks in advance and sorry for that many questions, but this process it is being a headache...



CostaIt is quite strange. *Check cas 5449-12-7 mp*. Also, you can take the solid orange "p2p oil" from your beaker (take couple grams) and dissolve in water at room temperature or with slight heating (about 30 deg C). I think that this solid is water soluble salt. If you'll get oily layer on the top, I am right.


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## Costa

Hi, as said, I repeated the process following the instructions of the document (and your comments) step by step. I got exactly the same product on this step:


 I took the oily layer (top layer, which has P2P) and once it cooled down after 10 minutes it has this aspect:

.

Then I added DCM over the other layer (the "water") in order to make the first extraction, however, this was the aspect of the mixture:


 

 

as you can see, there was some kind of white precipitate on the bottom, there were not two layers, just the white solids and the rest.
What did I do wrong? The document is not very clear... 
Many thanks in advance and sorry for that many questions, but this process it is being a headache...


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## G.Patton

Costa said:


> Hi, as said, I repeated the process following the instructions of the document (and your comments) step by step. I got exactly the same product on this step:View attachment 8916 I took the oily layer (top layer, which has P2P) and once it cooled down after 10 minutes it has this aspect:View attachment 8917.
> 
> Then I added DCM over the other layer (the "water") in order to make the first extraction, however, this was the aspect of the mixture:
> View attachment 8918 View attachment 8919 View attachment 8920as you can see, there was some kind of white precipitate on the bottom, there were not two layers, just the white solids and the rest.
> What did I do wrong? The document is not very clear...
> Many thanks in advance and sorry for that many questions, but this process it is being a headache...



CostaIt is quite strange. *Check cas 5449-12-7 mp*. Also, you can take the solid orange "p2p oil" from your beaker (take couple grams) and dissolve in water at room temperature or with slight heating (about 30 deg C). I think that this solid is water soluble salt. If you'll get oily layer on the top, I am right.


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