HRID2415436

反应详情

EQUATION

反应方程式

HRID 2415436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 6-(3-fluoro-benzyloxy)-3,4-dihydro-2H-isoquinolin-1-one (0.100 g, 0.369 mmol) and sodium hydride (55%, 22 mg, 0.51 mmol) in N,N′-dimethylformamide was heated at 70° C. for 1 h. Then ethyl-2-bromopropionate (0.072 mL, 0.55 mmol) was added and the resulting mixture was heated at 80° C. overnight. After cooling to room temperature, water was added and the reaction was extracted with dichloromethane. After drying of the organic layer with MgSO4, filtration and evaporation, the residue was purified by chromatography (SiO2, hexane/ethyl acetate 1:0 to 3:2 v:v gradient) to give the title compound as a white solid (0.095 g, 69%). MS: m/e=372.3 (M+H+).

WORKUP

后处理

  1. temperaturethe resulting mixture was heated at 80° C. overnight
  2. temperatureAfter cooling to room temperature
  3. extractionthe reaction was extracted with dichloromethane
  4. dry with materialAfter drying of the organic layer with MgSO4, filtration and evaporation
  5. customthe residue was purified by chromatography (SiO2, hexane/ethyl acetate 1:0 to 3:2 v:v gradient)