HRID1097243

反应详情

EQUATION

反应方程式

HRID 1097243 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of glycine (8.11 g, 108 mmol) in water (40 ml) were added an aqueous solution of sodium hydroxide (108 mmol, 15 ml) and a solution of 4-bromobenzaldehyde (20 g, 108 mmol) in methanol (240 ml). After 30 minutes stirring at room temperature sodium borohydride (4.09 g, 108 mmol) was added portionwise to this suspension. After 18 h stirring at room temperature the reaction mixture was concentrated under reduced pressure and the resulting aqueous phase was washed with diethyl ether. The aqueous phase was neutralized by the addition of an aqueous solution of 2M hydrochloric acid. The resulting precipitate was collected by filtration, washed with water and diethyl ether. Drying the white solid afforded 2-(4-bromobenzylamino)acetic acid (14.2 g). The product was used in the following step without further purification.

WORKUP

后处理

  1. additionwas added portionwise to this suspension
  2. concentrationwas concentrated under reduced pressure
  3. washthe resulting aqueous phase was washed with diethyl ether
  4. additionThe aqueous phase was neutralized by the addition of an aqueous solution of 2M hydrochloric acid
  5. filtrationThe resulting precipitate was collected by filtration
  6. washwashed with water and diethyl ether
  7. customDrying the white solid