G.Patton

Expert
Joined
Jul 5, 2021
Messages
2,411
Solutions
3
Reaction score
2,374
Points
113
Deals
1

D4mFCvyGwg

Introduction

Amphetamine can be obtained in a 30% yield in a one-step synthesis by refluxing phenylacetone in ethanol with ammonia, aluminium grit, and a small quantity of mercuric chloride. By trying out this reaction procedure for amphetamine, it was found that the yield of the reaction was not as high as for Pervitin (30% and 70%, respectively). However, the easiness of the procedure makes this method worthwhile. It's the simplest way to obtain amphetamine sulphate from P2P. Another way you can learn in Synthesis of Dextroamphetamine from P2P with (S)-(−)-α-Methylbenzylamine topic.

Equipment and glassware:

Reagents:

  • 40 g, 0.3 mole Phenylacetone (P2P) [CAS: 103-79-7];
  • 200 mL Ethanol (EtOH) 96-98 %
  • 200 mL 25 % Ammonia alc. (NH4OH);
  • 40 g, 1.5 moles Al-grit;
  • 0.3 g,1 mmol Mercury chloride (2) (HgCl2);
  • ~200 mL Distilled water;
  • 120 g Potassium hydroxide (KOH);
  • ~450 mL Diethyl ether (Et2O);
  • ~ 200 mL Hydrochloric acid 20 % (HCl) aq. solution;
  • ~ 200 g Sodium sulfate (Na2SO4);
  • ~30 mL Sulfuric acid conc. 98%.
18aQPG6yJ9
1-Phenyl-2-aminopropane sulfate:
Boiling Point (free base): 200-203 °C at 760 mm Hg;
Melting Point: 280-281 °C;
Molecular Weight: 368.5 g/mol;
Density: 0.936 g/mL;
CAS Number: 60-13-9.

Procedure

A mixture of 40 g (0.3 mole) phenylacetone, 200 mL ethanol, 200 mL 25 % ammonia, 40 g (1.5 mole) Al-grit and 0.3 g (1 mmol) HgCl2 is warmed with vigorous stirring in 2 L round bottom flask with reflux condenser until reaction takes place, after which warming is stopped immediately. Cooling should be applied if the reaction becomes too violent. When the violence of the reaction has diminished, the mixture is refluxed with vigorous stirring for about 2 h, concentrated in vacuo to 200 mL and poured into ice water, alkalinized with 120 g KOH, and extracted with ether (100 mL x 3). The extractions are treated with 20 % HCl, the resulting water layer alkalinized and extracted with 150 mL ether. The organic layer is dried over Na2SO4, the ether evaporated, and the residue distilled in vacuo. Yield: 12.5 g (30 %).
AgTpqxtUdZ
Preparation of amphetamine sulfate by addition of sulfuric acid drop-wise is yielded 96-98 % product with a purity of 99.2-99.8 % (USP grade), which was filtered as white powder on the Buchner flask and funnel and air dried. Here and here you can find video and photo-manuals of acidifying procedures respectively.
 
Last edited by a moderator:

GhostChemist

Expert
Joined
Nov 20, 2022
Messages
80
Reaction score
179
Points
33
The reactions proceed according to Scheme 1.
NbjWUpSrBQ

Equipment, Reagents and glassware for the 1st and 2nd experiments:

  • 10.5 grams of 14μm aluminum foil
  • 0.1 grams of mercury chloride
  • 50 mL of 20-25% ammonia
  • 10 grams of sodium chloride in 30 mL of water
  • 10 grams of purified P2P and 10 grams of unpurified P2P (P2P obtained through the reduction of P2NP with sodium borohydride)
  • 100-150 mL of 88% ethanol
  • 150-200 mL of DCM (dichloromethane)
  • 3-5 mL of concentrated sulfuric acid (80%)
  • pH indicator paper
  • 2 liters of technical-grade water with 500 grams of ice
  • 20-30 grams of anhydrous sodium sulfate
  • 10-15 mL of 25% NaOH (sodium hydroxide)
  • 35-40 mL of acetone
  • 2-liter, 500 mL, and 250 mL flasks
  • Condenser
  • Solvent distillation setup with a water bath
  • Vacuum filtration setup
  • Separatory funnel
  • Silicone grease for grinding
  • Filter paper
  • Funnels
  • Beakers
  • Heater

Stage 1. Aluminum amalgam formation.
Two liters of water are poured into a flask, and aluminum foil is added so that it is submerged beneath the water. Dry mercury chloride is added, and the mixture is vigorously stirred until active hydrogen evolution occurs and a dullness appears on the foil (approximately 10-15 minutes).
Fig 1
ANueSvskFo


Fig 2

Tq2CiBcKWD

Next, the solution is drained, and the aluminum amalgam is rinsed twice with distilled water.

Purified P2P Fig 3

XdeAOCQVuD


Unpurified P2P Fig 3.1
WxOPi7N1GE


Stage 2. Reduction and extraction.
Preparation of ice-cold water for cooling the flask should be done in advance. Water ammonia, sodium chloride solution, P2P, and ethanol are added to the obtained aluminum amalgam. The reflux condenser is connected. The exothermic reaction begins after 5-10 minutes with pure P2P and almost instantaneously with impure P2P.
Fig 4

MxYE6LojQl


The reactor should be cooled if the temperature exceeds 50-60 ℃.
Fig 5

YhIuBKSLiZ


The reaction fully takes place in approximately 30-40 minutes. During this time, the reagents transform into a gray mass.
Fig 6
7fKFci1ksW


To the reaction mass, 10-15 ml of 25% NaOH is added to dissolve any unreacted aluminum, and it is left to stand for 30-40 minutes until the hydrogen evolution ceases.
Fig 7
HQb6PsVv28


After the alkaline solution is added and the hydrogen gas evolution is complete, the mixture is allowed to settle for approximately 1 hour and then filtered.
Fig 8
XBqSd6AT3N


Filtered solution obtained from purified P2P.
Fig 9

QBUMIRZD5z


Filtered solution obtained from impure P2P.
Fig 10

AgIialjShz


50-100 mL of dichloromethane is added to the filtered solution.
Fig 11

Bzq1In0s4o


The resulting emulsion is transferred in several portions to a separatory funnel and allowed to settle. The layer of dichloromethane is separated, and additional portions of dichloromethane are used for further extraction.
Fig 12

QG9hxbFjtO

The extract in dichloromethane (purified P2P).
Fig 13
H0qxGIHJ6k


The extract in dichloromethane (impure P2P).
Fig 14
IYsqFkXLPj


The separated layer of dichloromethane is dried over anhydrous sodium sulfate and, if necessary, filtered.
Fig 15
ObIg9pDn61


The dried layer of dichloromethane is transferred to a flask for distillation. The dichloromethane is completely distilled off until a temperature of 90°C is reached.
Fig 16

S3upWDb1By


The residue after the distillation of dichloromethane (purified P2P).
Fig 17

9tVRwDXx3r


The residue after the distillation of dichloromethane (impure P2P).
Fig 18

RUzV1SZhg9


To the obtained amine, 10-15 mL of acetone is added, and concentrated sulfuric acid is slowly added until the pH reaches 5.5-6. Then, the resulting solution is evaporated until crystallization occurs.
Fig 19
IlHiVK7G6T


The crystallized mass is mixed with 15-20 mL of cold acetone, thoroughly stirred, and transferred onto a vacuum filter. It is further washed with a portion of cold acetone and dried directly on the filter or under a stream of warm air.
Fig 20
RlPwOZsdg6


Fig 21

OdskljfWRy


The powder is the amphetaminesulfate obtained from purified P2P.
Fig 22

Jl83ZhSKcH


The powder is the amphetaminesulfate obtained from unpurified P2P.
Fig 23
BomRAsnwvO


In theory, from 10 g of P2P, it should be possible to obtain 10.077 g of amphetamine in the form of a base with 100% conversion. From 10.077 g of amphetamine as a base, theoretically, it should be 1/2 mole of sulfate or 13.73 g of amphetamine sulfate.

From pure P2P, 5.65 g of amphetaminesulfate was obtained, which corresponds to 41.1% yield.

From impure P2P, 2.29 g of amphetaminesulfate or 16.68% yield was obtained.


Conclusions
The yield of amphetaminesulfate using impure P2P is nearly 2.5 times lower than when using purified P2P. Such yields are likely due to the presence of impurities with double bonds, which locally enhance the exothermic effect of the reaction, leading to the evaporation of ammonia from the reaction volume (ammonia is lighter than air, unlike methylamine). Taking into account the obtained experimental data, it is more reasonable to use P2P in the production of methamphetamine.
 

Mr.Blanks00

Don't buy from me
Resident
Joined
Sep 2, 2022
Messages
43
Reaction score
17
Points
8
hello sir, sorry i want to ask. I have made amphetamines in this way I get a layer of oil as much as 25 grams and when I make sulfate salt I get 8 grams, while from the solution I extract it and get only 1 gram, is this appropriate or not sir, sorry sir 1 more for how to use this amphetamine how many mg for the moderate dose and how do you use it, is it a pill or what, sir, please advise sir, thank you.
 

G.Patton

Expert
Joined
Jul 5, 2021
Messages
2,411
Solutions
3
Reaction score
2,374
Points
113
Deals
1
hello sir, sorry i want to ask. I have made amphetamines in this way I get a layer of oil as much as 25 grams and when I make sulfate salt I get 8 grams, while from the solution I extract it and get only 1 gram, is this appropriate or not sir, sorry sir 1 more for how to use this amphetamine how many mg for the moderate dose and how do you use it, is it a pill or what, sir, please advise sir, thank you.
YusufHello, 9g in total is to small (~21% conversion). How much P2P have you used? Probably you got 25 g not pure amphetamine free base or I didn't understand your text clearly.
how to use this amphetamine how many mg for the moderate dose and how do you use it, is it a pill or what, sir, please advise sir, thank you.
You can open BB Wiki ==> Amphetamine and read about.
 

Mr.Blanks00

Don't buy from me
Resident
Joined
Sep 2, 2022
Messages
43
Reaction score
17
Points
8
I used 40gram p2p , I got 25gram free base oil, but when I made sulfate salt I only got 8gram.
 

G.Patton

Expert
Joined
Jul 5, 2021
Messages
2,411
Solutions
3
Reaction score
2,374
Points
113
Deals
1
I used 40gram p2p , I got 25gram free base oil
YusufIt is quite good yield, 62.5%. I think there is not pure amphetamine free base. You can check boiling point of your oil. If it is very different from amphetamine, you can vacuum distill it.
 

studentt

Don't buy from me
Resident
Joined
Jul 29, 2022
Messages
17
Reaction score
8
Points
3
hello, i have freebase a-oil but i have some problems. it is crystal clear but the ph is 11.8. and it also smell like caustic. what should i do to purefy it. i have done normale distillation because i can reach high temperature. should i wash it with boiling water?
 

G.Patton

Expert
Joined
Jul 5, 2021
Messages
2,411
Solutions
3
Reaction score
2,374
Points
113
Deals
1

studentt

Don't buy from me
Resident
Joined
Jul 29, 2022
Messages
17
Reaction score
8
Points
3
above 200c. i don’t know exactly because my heatingmantle is without display. but when i distilled it. reach the boiling ponit it was something like gas. and turn back to liquid.
 

G.Patton

Expert
Joined
Jul 5, 2021
Messages
2,411
Solutions
3
Reaction score
2,374
Points
113
Deals
1
above 200c. i don’t know exactly because my heatingmantle is without display. but when i distilled it. reach the boiling ponit it was something like gas. and turn back to liquid.
studenttBoiling point is indirect confirmation of substance purity. You can read here to understand it clearly Boiling point determination. The thermometer must be used for distillation purposes.
 

blackburn

Don't buy from me
Resident
Joined
Aug 18, 2022
Messages
107
Reaction score
44
Points
28
at what scale can this synthesis be done in? is there any other process when it comes to around 1l p2p
 

G.Patton

Expert
Joined
Jul 5, 2021
Messages
2,411
Solutions
3
Reaction score
2,374
Points
113
Deals
1
at what scale can this synthesis be done in? is there any other process when it comes to around 1l p2p
SwesweI think reaction will be too violent and a yield will be decreased. I'm not sure that you can scale it more than 100g.
 

blackburn

Don't buy from me
Resident
Joined
Aug 18, 2022
Messages
107
Reaction score
44
Points
28
I think reaction will be too violent and a yield will be decreased. I'm not sure that you can scale it more than 100g.
G.Pattonok thanks for reply! Do you know which route is best for larger batches? I've looked a bit at P2NP with NaBH4/CuCl2 (1kg scale) but I'm also looking for bigger than that if there's a possibility, sorry for asking here, know it doesn't belong in the thread

/Regards
 

Gale

Don't buy from me
Resident
Joined
Mar 30, 2022
Messages
85
Reaction score
48
Points
18
How much mercuric chloride you guys reccomend for 800g synth
 

Hank Schrader

Don't buy from me
Resident
Joined
Nov 10, 2022
Messages
72
Reaction score
150
Points
33
hello sir, how do you use anhydrous ammonia while the hgcl reaction must contain water content.. can you explain your method.
YusufIt's that simple. The technology has long been known, which uses an autoclave and anhydrous ammonia. The ammonia cylinder is connected to the autoclave and saturated with the icy methanol to the desired mass. Usually make a 10-12% solution of ammonia in methanol. Water will of course be in small quantities in the reaction because when imine is formed, the reaction releases water...
Amphetamine can be obtained both on aluminum and on other catalysts, but in the case of using Raney or other metals, hydrogen must be supplied to the reaction.
 
  • Free product samples

    Testing products from new vendors and manufacturers.

    Get free samples for testing now!

  • Always stay in touch with BB forum. Element/Matrix.

    Connect notifications to always stay in touch with the forum!

    Connect

  • The BB Forum team is looking for cooperation:

    • Traffic arbitrage specialists
    • Spammers
    • Advertising agencies
    • Bloggers/Vloggers
    • TOR sites directories
    • Creative people who can create viral content
    • Administrators of Telegram Channels and Groups

      We will pay more for your traffic than our competitors! $0.1 per visitor!!!If you are interested in, write to the administrator.
Top