HRID49418

反应详情

EQUATION

反应方程式

HRID 49418 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 N-(3-trifluoromethylphenyl)-N′-(2-ethyloxycarbonylphenyl)-1,2-diaminoethane (1.1 g, 3.1 mmol) and triethylamine (1.1. mL, 7.5 mmol) in toluene was added phosgene in toluene (1.84 mL, 3.5 mmol). After stirring at room temperature for 30 min. Water and diethyl ether were added. The organic phase was dried and evaporated to dryness. The resulting residue was purified by column chromatography on silica gel using dichloromethane as eluent. The isolated ester (0.96 g) was hydrolysed in 4N aqueous sodium hydroxide to give the desired compound in a yield of 0.6 g. M.p. 197-198° C.

WORKUP

后处理

  1. customThe organic phase was dried
  2. customevaporated to dryness
  3. customThe resulting residue was purified by column chromatography on silica gel