反应详情

9.6 g of 3-amino-3-(4-chlorophenyl)propionic acid are dissolved in 200 ml of dioxane and about 50 ml of 1N NaOH in order to reach pH=10.5-11.5. The medium is cooled to +5° C. and 6.34 ml of phenylacetyl chloride are then gradually added, while maintaining the mixture at pH=10.5-11.5 and at a temperature of between +5° C. and +10° C.. Stirring is continued for 1 and a half hours and the medium is then concentrated to one-half before diluting with 500 ml of water. The resulting mixture is washed twice with EtOAc and then acidified to pH=1-2 by addition of 6N HCl The solid is drained, washed with water and dried to give 14 g of the expected compound.

1. temperatureThe medium is cooled to +5° C.
2. temperaturewhile maintaining the mixture at pH=10.5-11.5
3. customat a temperature of between +5° C. and +10° C.
4. customis continued for 1 and a half hours
5. concentrationthe medium is then concentrated to one-half
6. additionbefore diluting with 500 ml of water
7. washThe resulting mixture is washed twice with EtOAc
8. additionacidified to pH=1-2 by addition of 6N HCl The solid
9. washwashed with water
10. customdried