反应详情

温度

28 °C

150 g N-[(2′-cyanobiphenyl-4-yl)methyl]-(L)-valine methyl ester hydrochloride was charged into a round bottomed flask containing a mixture of sodium bicarbonate (158.1 g), water (450 ml) and toluene (900 ml). The contents were stirred at 28° C. for 25 minutes and then cooled to 0° C. 110.9 g of valeryl chloride was added slowly to the reaction mass at 0-20° C. over about 55 minutes. The reaction mass was stirred at about 2-4° C. for about 2 hours. Reaction completion was confirmed by thin layer chromatography and the reaction mixture was allowed to attain 28° C. 450 ml of water was added to the reaction mass and stirred for about 20 minutes. The organic layer was separated, washed with a solution of sodium bicarbonate (30 g) in water (450 ml) twice, followed by washing with water (450 ml). The organic layer was concentrated under reduced pressure at 60-68° C. to obtain 183 g of the title compound.

1. additioncontaining
2. temperaturecooled to 0° C
3. stirringThe reaction mass was stirred at about 2-4° C. for about 2 hours
4. customReaction completion
5. customto attain 28° C
6. stirringstirred for about 20 minutes
7. customThe organic layer was separated
8. washwashed with a solution of sodium bicarbonate (30 g) in water (450 ml) twice
9. washby washing with water (450 ml)
10. concentrationThe organic layer was concentrated under reduced pressure at 60-68° C.