HRID1034063

反应详情

EQUATION

反应方程式

HRID 1034063 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A solution of 3-(3-nitrobenzyl)indole (280 mg) in N,N-dimethylforma/nide (5 ml) was added to a suspension of sodium hydride (60% dispersion in mineral oil, 66.6 mg) in N,N-dimethylformamide (10 ml) at 0° C. The mixture was stirred at 25° C. for 40 minutes, and a solution of benZyl phenyl succinate (316 mg) in N,N-dimethylformamide was added at -40° C. After stirred at -40° C. for 20 minutes, the reaction mixture was poured into a mixture of ethyl acetate and 1N hydrochloric acid. The organic layer was separated, washed with water and brine, and dried over, magnesium sulfate. After evaporation of the solvent, the crude crystals were washed with hot isopropyl ether to give benzyl 4-[3-(3-nitrobenzyl)indol-l-yl]-4-oxobutyrate (364 mg).

WORKUP

后处理

  1. stirringAfter stirred at -40° C. for 20 minutes
  2. customThe organic layer was separated
  3. washwashed with water and brine
  4. dry with materialdried over, magnesium sulfate
  5. customAfter evaporation of the solvent
  6. washthe crude crystals were washed with hot isopropyl ether