HRID1836135

反应详情

EQUATION

反应方程式

HRID 1836135 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Triethylamine (146 μl, 1.0 mmol) was added to 3-(3-piperazin-1-yl-propyl)-4,5,6,7-tetrahydro-1H-indole-2-carbaldehyde (192 mg, 0.7 mmol) in 5 ml of dimethylformamide at 0° C. Ethyl chloroformate (87 μl, 0.91 mmol) was dropped in the mixture. The reaction mixture was stirred at 0° C. which was raised slowly to room temperature over night. Thin layer chromatography (dichloromethane: methanol 10:1) showed on major spot. The solvent was evaporated then the residue was purified by flash chromatography and eluting with (dichloromethane/methanol =50/1, 40/1, 30/1) to give 130 mg of 4-[3-(2-formyl-4,5,6,7-tetrahydro-1H-indol-3-yl)-propyl]-piperazine-1-carboxylic acid ethyl ester.

WORKUP

后处理

  1. temperaturewas raised slowly to room temperature over night
  2. customThe solvent was evaporated
  3. customthe residue was purified by flash chromatography
  4. washeluting with (dichloromethane/methanol =50/1, 40/1, 30/1)