HRID1836135
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas raised slowly to room temperature over night
- customThe solvent was evaporated
- customthe residue was purified by flash chromatography
- washeluting with (dichloromethane/methanol =50/1, 40/1, 30/1)