HRID1878390

反应详情

EQUATION

反应方程式

HRID 1878390 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A stirred mixture of (3-fluoro-4-nitrophenyl)(3-(fluoromethyl)piperazin-1-yl)methanone (456 mg, 1.6 mmol), N-tert-butyl-3-(chloromethyl)benzamide (361 mg, 1.6 mmol), triethylamine (3.1 mmol, 341 mg) and sodium iodide (1.6 mmol, 240 mg) in acetonitrile (10 mL) was heated to 60° C. for several hours. The reaction was concentrated under reduced pressure. The residue was then dissolved in dichloromethane and extracted with water (×3). The organic phase was dried (sodium sulfate) and concentrated under vacuum. The crude material was purified using silica chromatography to give the title compound (435 mg). MS (ESI) m/z 475.7[M+H]+

WORKUP

后处理

  1. concentrationThe reaction was concentrated under reduced pressure
  2. dissolutionThe residue was then dissolved in dichloromethane
  3. extractionextracted with water (×3)
  4. dry with materialThe organic phase was dried (sodium sulfate)
  5. concentrationconcentrated under vacuum
  6. customThe crude material was purified