One Step Dextroamphetamine Synthesis

G.Patton

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Introduction

The method have developed for the manufacture of amphetamine, that avoids the use of bases, avoids the use of toxic and dangerous reagents, requires mild reaction conditions, produces essentially no by-products or impurities in the final products thereby eliminating the need for separate purification steps, is short, does not use controlled substances, is very robust and is Suited to large-scale manufacture. This method also takes advantage of the innate stereochemistry of the starting materials, thereby eliminating the need for resolution steps.

Equipment and glassware:
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  • Three necked round bottom flask 150 mL;
  • pH indicator papers;
  • Beakers (100 mL x2, 1 L, 250 mL x2);
  • Laboratory scale (1-100 g is suitable);
  • Ice/water bath;
  • Glass rod and spatula;
  • Laboratory grade thermometer;
  • Buchner flask and funnel;
  • Hirsch funnel;
  • Filter paper;
  • TLC plate;
  • Celite;
  • Drip funnel;
  • Hydrogen gas (H2) source;
  • Balloon;

Reagents:
  • (4S,5R)-(-)-4-methyl-5-phenyl-2-oxazolidinone 6.00 g (33.9 mmol);
  • Palladium on-carbon (50% water wet) 10% 0.34 g;
  • SDA-3A (a solvent constituting 95% Ethanol and 5% Methanol) 60 mL;
  • Sulphuric acid (H2SO4 (aq)) 25% ~7 mL;
  • Isopropyl alcohol IPA (or ether);
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Procedures

1. A mixture of 6.00 g (33.9 mmol) (4S,5R)-(-)-4-methyl-5-phenyl-2-oxazolidinone, 0.34 g 10% palladium on-carbon (50% water wet), and 60 mL SDA-3A (a solvent constituting 95% Ethanol and 5% Methanol) is stirred in a three necked 150 mL round bottom flask under a hydrogen filled balloon at ambient temperature (approximately 20°C) until no more oxazolidinone was detected by TLC, ~4h.
2. The reaction mixture is then filtered through a pad of Celite on a Hirsch funnel to remove the catalyst.
3. Whereupon a total of 7 mL 25% H2SO4 (aq) was added dropwise to the filtrate over 3 min to a neutral pH.
4. After cooling in an ice/water bath for 15 min, the mixture is filtered to collect the dextroamphetamine sulfate using cold dry IPA (or ether) as a flask and cake rinse.
5. After drying, a total of 5.79 g of dextroamphetamine sulfate is obtained, 93% yield. This material is assayed at 100% by HPLC.
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Source

United States (12) Patent Application Publication US 2010.01251.46A1
 

Mo0odi

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I hope you make a video this way

Thank you
 

handle

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Can an 'Adams catalyst' be used instead of Palladium on-carbon?
Pd/C is hard to source here.
 

ZMI_AA0B

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Idol, is synthetic methamphetamine sulfate a finished product of methamphetamine
 

Pororo

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Awesome.
CAS 16251-45-9. Available in Europe?
 

Frit Buchner

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It looks like you took aminorex and turned it into methamphetamine? If I could get that chemical I would probably make something else
 

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It looks like you took aminorex and turned it into methamphetamine? If I could get that chemical I would probably make something else
Frit Buchneris it aminorex? it looks more it belongs to antibiotic group.
 

G.Patton

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G.Patton

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What is product name made from this cas? Probably antibiotic. Easy to find on common market?
PororoThe name is written in this topic in Reagents. I have no data about current situation with this reagent.
 

Pororo

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The name is written in this topic in Reagents. I have no data about current situation with this reagent.
G.PattonSure i'm not such a stupid to ask about "(4S,5R)-(-)-4-methyl............." Name i mean ready product name, the same as "aminorex" for example. Brief search doesn't give any result, but it looks as a kind of antibiotic.
 

Frit Buchner

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noMoneynoHoney234

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1. 6.00 g (33.9 mmol) (4S,5R)-(-)-4-甲基-5-苯基-2-噁唑烷酮、0.34 g 10% 鈀碳(50% 水潤濕)和60的混合物將mL SDA-3A(由95%乙醇和5%甲醇組成的溶劑)在充滿氫氣的氣球下在三頸150mL圓底燒瓶中在環境溫度(約20℃)下攪拌直至通過TLC不再檢測到噁唑烷酮, 〜4小時。
G.PattonSir,Is there any way to replace hydrogen?Can NaBH4 be used?
 

handle

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Kinda sucks when the reagents are more expensive than the end product.
Product: (4S,5R)-(-)-4-METHYL-5-PHENYL-2-OXAZOLIDINONE
Quantity: 5kg
Price: USD $8597.00
 

Pororo

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Kinda sucks when the reagents are more expensive than the end product.
Product: (4S,5R)-(-)-4-METHYL-5-PHENYL-2-OXAZOLIDINONE
Quantity: 5kg
Price: USD $8597.00
handleChinese offer it for 500$ per 1 kg. But purity could be questionable.
 

Pororo

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Kinda sucks when the reagents are more expensive than the end product.
Product: (4S,5R)-(-)-4-METHYL-5-PHENYL-2-OXAZOLIDINONE
Quantity: 5kg
Price: USD $8597.00
handleFrom 1 kg you may get 1320 gr of D-amph sulphide pharma grade (if prec is OK). Is it bad yield?

But meth prec Ephedroxane may be not such an easy shit to get.
CAS16251-46-0
__pubchem.ncbi.nlm.nih.gov/compound/Ephedroxane
 
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