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G.Patton

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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
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Equipment and glassware:

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);
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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.
 

Saul

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We forget ~20 g NaOH or KOH; and this is your first step.

Anyway, My p2p was really perfect, also a great yield. And very beautiful almost fluorescent yellow
500 gr BMK methylglycidate I add VERY slowly in a liter of 80°c sulfonic acid (NO WATER)
it takes 30 min
I start with reflux after and the temperature rises from 80°c to 145°c
I use a very powerful mixer. 3 hours later it is ready to cool down take the top layer 285ml
and I'll save the bottom layer for the next time you can use it again with no problem, exactly the same yield.
I'm trying 70/30 the third attempt, so only 300ml new sulfonic acid and 700ml used.
And the fourth time I used all 1000 ml used and exactly the same yield. ph0.5
I don't think this was possible if I started with NaOH? I don't know because I didn't do it.
 
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Saul

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

G.Patton

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edit // VERY slowly in a liter of 80°c phosphoric acid (NO WATER)
Do you use H3PO4 cons or diluted solution? Thank you for your feedback.
 

Saul

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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 )
 

KokosDreams

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I use a very powerful mixer.
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
 

Saul

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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

yes no problem
 

Saul

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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 )
 

KokosDreams

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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 )
No 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?
 

Saul

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no its fine !
 

G.Patton

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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 )
I asked about acid solution. :unsure:
 

jasper12

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

Jesse_Pinkman_

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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

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

Heating Mantles are a great addition for any lab!
 

Jesse_Pinkman_

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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

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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
Exciting :) Good luck!
 
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