HRID844307

反应详情

EQUATION

反应方程式

HRID 844307 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of [3-chloro-4-(3-dimethylamino-acryloyl)-phenyl]-carbamic acid tert-butyl ester (250 mg) in ethanol (1.25 ml) is treated with hydrazine hydrate (0.25 ml) and the mixture is stirred at room temperature for 3 hours. The mixture is then diluted with 30 mL of diethyl ether, washed three times with water, once with saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate. The solvent is removed by evaporation under reduced pressure and the resulting residue is chromatographed over silica gel (67% ethyl acetate in hexanes is used as the eluant) to provide the desired product as an oil.

WORKUP

后处理

  1. washwashed three times with water
  2. dry with materialonce with saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate
  3. customThe solvent is removed by evaporation under reduced pressure
  4. customthe resulting residue is chromatographed over silica gel (67% ethyl acetate in hexanes