Process for the purification of benzphetamine hydrochloride
View Patent ↗The present invention relates to the economical and separation of benzphetamine hydrochloride and methamphetamine by liquid extraction. An extraction process employing a suitable organic solvent and water at a pH in the range of from about 6 to about 8 provides excellent removal of the methamphetamine by dissolution in the water phase while the benzphetamine dissolves in the organic phase. Simple separation of the two phases results in separation of the two amines.
1. A process for removing methamphetamine hydrochloride from crude benzphetamine hydrochloride which comprises subjecting the said crude hydrochlorides to liquid extraction with an organic solvent and water at a pH in the range of from about 6 to 8 wherein the benzphetamine hydrochloride is converted to a base and separates into the organic phase and the methamphetamine hydrochloride remains in the aqueous phase.
2. The process of claim 1 wherein the pH is in the range of from about 6 to about 6.5.
3. The process of claim 1 wherein the organic solvent selected from the group consisting of benzene, toluene, xylene, hexane, heptane, cyclohexane.
4. The process of claim 3 wherein organic solvent is toluene.
5. The process of claim 1 wherein the pH of the water is adjusted with an acid.
6. The process of claim 5 wherein the acid is selected from the group consisting of hydrochloric acid, sulfuric acid, phosphoric acid, and acetic acid.
7. The process of claim 6 wherein the acid is hydrochloric acid.
8. The process of claim 1 wherein the pH of the water is adjusted with a base.
9. The process of claim 8 wherein the base is selected from the group consisting of alkali metal carbonates, alkali metal bicarbonates and alkali metal hydroxides.
10. The process of claim 9 wherein the base is sodium carbonate.
11. A process for removing methamphetamine from crude benzphetamine hydrochloride which comprises the steps of:
A. subjecting the crude benzphetamine hydrochloride to liquid extraction with an organic solvent and water at a pH in the range of from about 6 to 8;
B. separating the water containing the methamphetamine base from the organic solvent containing benzphetamine base, then converting the benzphetamine base to the hydrochloride salt; and
C. separating the benzphetamine hydrochloride salt from the organic solvent.
12. The process of claim 11 wherein step C is performed by filtration of the benzphetamine hydrochloride salt from the organic solvent.
13. The process of claim 11 wherein step C is performed by extracting benzphetamine hydrochloride salt from the organic solvent.
14. The process of claim 11 wherein the pH of the water in step A is in the range of from about 6 to about 6.5.
15. The process of claim 11 wherein the organic solvent selected from the group consisting of benzene, toluene, xylene, heptane and cyclohexane.
16. The process of claim 15 wherein organic solvent is toluene.
17. The process of claim 11 wherein the pH of the water is adjusted with an acid.
18. The process of claim 17 wherein the acid is selected from the group consisting of hydrochloric acid, sulfuric acid, phosphoric acid and acetic acid.
19. The process of claim 18 wherein the acid is hydrochloric acid.
20. The process of claim 11 wherein the pH of the water is adjusted with a base.
21. The process of claim 20 wherein the base is selected from the group consisting of alkali metal hydroxides, alkali metal carbonates and alkali metal bicarbonates.
22. The process of claim 21 wherein the base is selected from the group consisting of sodium hydroxide, potassium hydroxide; sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate.
23. The process of claim 22 wherein the base is sodium carbonate.
24. A process for removing methamphetamine hydrochloride from crude benzphetamine base which comprises subjecting crude methamphetamine base and the benzphetamine base to liquid extraction with an organic solvent and water at a pH in the range of from about 6 to 8 wherein the benzphetamine base remains in the organic phase and the methamphetamine is converted to a salt and remains in the aqueous phase.
25. The process of claim 24 wherein the pH is in the range of from about 6 to about 6.5.
26. The process of claim 24 wherein the organic solvent selected from the group consisting of benzene, toluene, xylene, hexane, heptane, cyclohexane.
27. The process of claim 26 wherein organic solvent is toluene.
28. The process of claim 24 wherein the pH of the water is adjusted with an acid.
29. The process of claim 28 wherein the acid is selected from the group consisting of hydrochloric acid, sulfuric acid, phosphoric acid, and acetic acid.
30. The process of claim 29 wherein the acid is hydrochloric acid.
31. The process of claim 24 wherein the pH of the water is adjusted with a base.
32. The process of claim 31 wherein the base is selected from the group consisting of alkali metal carbonates, alkali metal bicarbonates and alkali metal hydroxides.
33. The process of claim 32 wherein the base is sodium carbonate.