HRID77514

反应详情

EQUATION

反应方程式

HRID 77514 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.0 g (4.65 mmol) alpha-bromophenylacetic acid (Aldrich), 1.16 g (6.05 mmol) (3-dimethylamino-propyl)-ethyl-carbodiimide hydrochloride (Aldrich), 2.80 mL (5.6 mmol) ethyl-amine (Aldrich, 2 M in dichloromethane) in dichloromethane (30 mL) is stirred at room temperature for 18 h. The reaction mixture is washed with NaOH 1 M (15 mL) and the organic phase is evaporated under reduced pressure. The residue is purified by silica gel column chromatography (gradient: cyclohexane/ethyl acetate 90:10 to 50:50) to yield the title compound (0.32 g, content ca. 90%).

WORKUP

后处理

  1. washThe reaction mixture is washed with NaOH 1 M (15 mL)
  2. customthe organic phase is evaporated under reduced pressure
  3. customThe residue is purified by silica gel column chromatography (gradient: cyclohexane/ethyl acetate 90:10 to 50:50)