反应详情

温度

30 °C

20 g of 2-(N-benzyl-N-(2-hydroxyethyl) amino)-2-(4-fluorophenyl) acetamide of Formula X, 200 ml of acetone and 10 g of L-(+)-tartaric acid were charged in a clean and dry 4 neck round bottom flask. The resultant reaction suspension was heated to reflux followed by stirring for about 3 hours. The reaction solution was cooled to about 30° C. followed by filtration of the solid and the solid was washed with 40 ml of acetone. Filtrate was distilled completely at about 50° C. under vacuum, to the residue 200 ml of dichloromethane, 30 ml of water and 3 g of sodium carbonate were charged followed by stirring for about 15 minutes. Organic and aqueous layers were separated and the organic layer was washed with 30 ml of water. Organic and water layer were separated and 70% of the solvent on the total volume was distilled at about 45° C. under vacuum followed by addition of 10 ml of dilute hydrochloric acid. The resultant acidified organic layer was distilled completely at about 45° C. under vacuum. 100 ml of acetone was charged to the residue and was stirred for about 30 minutes. Separated solid was filtered and the solid was washed with 40 ml of acetone. The resultant wet solid was charged in a clean and dry 4 neck round bottom flask followed by charging of 200 ml of dichloromethane, 30 ml of water and 3 g of sodium carbonate. Resultant reaction suspension was stirred for about 15 minutes, followed by separation of organic and aqueous layers. Organic layer was washed with 30 ml of water. Organic and water layers were separated and the organic layer was distilled completely at about 40° C. under vacuum to yield 16 g of the title compound.

1. customdry 4 neck round bottom flask
2. customThe resultant reaction suspension
3. temperaturewas heated
4. temperatureto reflux
5. filtrationfollowed by filtration of the solid
6. washthe solid was washed with 40 ml of acetone
7. distillationFiltrate was distilled completely at about 50° C. under vacuum, to the residue 200 ml of dichloromethane, 30 ml of water and 3 g of sodium carbonate
8. additionwere charged
9. stirringby stirring for about 15 minutes
10. customOrganic and aqueous layers were separated
11. washthe organic layer was washed with 30 ml of water
12. customOrganic and water layer were separated
13. distillation70% of the solvent on the total volume was distilled at about 45° C. under vacuum
14. additionfollowed by addition of 10 ml of dilute hydrochloric acid
15. distillationwas distilled completely at about 45° C. under vacuum
16. addition100 ml of acetone was charged to the residue
17. stirringwas stirred for about 30 minutes
18. customSeparated solid
19. filtrationwas filtered
20. washthe solid was washed with 40 ml of acetone
21. additionThe resultant wet solid was charged in a clean and
22. customdry 4 neck round bottom flask
23. customResultant reaction suspension
24. stirringwas stirred for about 15 minutes
25. customfollowed by separation of organic and aqueous layers
26. washOrganic layer was washed with 30 ml of water
27. customOrganic and water layers were separated
28. distillationthe organic layer was distilled completely at about 40° C. under vacuum