(+/-)-METHADONE synthesis
- Product Name:(+/-)-METHADONE
- CAS Number:76-99-3
- Molecular formula:C21H27NO
- Molecular Weight:309.45
Yield:76-99-3 110.5 g
Reaction Conditions:
Stage #1:(R,S)-2,2-diphenyl-4-dimethylaminopentanenitrile;ethylmagnesium bromide in 5,5-dimethyl-1,3-cyclohexadiene;diethyl ether at 25 - 115;
Stage #2: with hydrogenchloride;water at 80 - 90;
Steps:
2 A process to produce 6-(dimethylamino)-4,4-diphenylheptan-3-one
1. Charge 310 ml dry ether under room temperature ranging from 18°C to 23°C. 2. Charge solution of ethyl magnesium bromide (prepared from 19.54gm magnesium and 84.66gm ethyl bromide) for at least 20-30 minutes at a temperature ranging from 25°C to 30°C. 3. Next, charged lOOmI solution into 190 ml xylene. Mix for at least 15 minutes. 4. Remove solvent from reaction mixture by distillation at a temperature ranging from 40°C to 80°C. 5. Conduct a ref lux for at least 240 minutes at a temperature ranging from 110°C to 115°C. 6. Next, charge 154.47m1 of concentrated hydrochloric acid at a temperature ranging from 80°C to 90°C. Then, charge 155m1 demineralised water. 7. Remove solvent by distillation at a temperature ranging from 110°C to 115°C. 8. Allow to cool at a temperature ranging from 18°C to 23°C. 9. Stir for at least 60 minutes. 10. Filter the solid, wash with 1:1 hydrochloric acid (50m1). 11. Dry the solid using vacuum pressure? 12. Add 350ml methanol to allow re-crystallization of the solid. 13. Finally, remove excess solvent and dry the solid under reduced pressure by vacuum drying at a temperature ranging from 50°C to 55°C and at a pressure of 40 to 45 psi. Results: • Wetwt: 128.38gm • Drywt:110.5Ogm • Yield:1.lOw/w
References:
UNIVERSITI SAINS MALAYSIA;ISMAIL, Rusli;ALI, Asaraf;TAN, Soo Choon WO2013/77720, 2013, A1 Location in patent:Page/Page column 4; 5; 8
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