反应详情

(c)Preparation of (R)—N-piperidin-3-ylacetamide Dibenzyol tartarate salt: In a RBF charged 500 ml of Methanol, 50 gm of N-piperidin-3-ylacetamide & 138 gm of L (+)-Dibenzoyl tartaric acid. The reaction was maintained for about 90 mins at room temperature and then heated to reflux. The reaction mass was maintained for about an hour at reflux and then cooled and maintained at room temperature for about 12.0 hours. Then, the product was filtered and washed with 100 ml methanol. Again charged the obtained wet cake in 800 ml methanol, heated to reflux and maintained reaction mass for 1.0 hr to get a clear solution. Cooled the reaction mass to room temperature and maintained for 12.0 hrs. The product was filtered and washed with 100 ml methanol. The product was dried at about 45-50° C. under vacuum. Unwanted S-isomer NMT 1.5% Dry Wt-20. Gm.

1. temperatureheated to reflux
2. temperatureThe reaction mass was maintained for about an hour
3. temperatureat reflux
4. temperaturecooled
5. temperaturemaintained at room temperature for about 12.0 hours
6. filtrationThen, the product was filtered
7. washwashed with 100 ml methanol
8. additionAgain charged the obtained wet cake in 800 ml methanol
9. temperatureheated
10. temperatureto reflux
11. temperaturemaintained
12. customreaction mass for 1.0 hr
13. customto get a clear solution
14. temperatureCooled the reaction mass to room temperature
15. temperaturemaintained for 12.0 hrs
16. filtrationThe product was filtered
17. washwashed with 100 ml methanol
18. customThe product was dried at about 45-50° C. under vacuum
19. customUnwanted S-isomer NMT 1.5% Dry Wt-20