HRID1160454

反应详情

EQUATION

反应方程式

HRID 1160454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of methyl 3-bromo-5-[methyl(methylsulfonyl)amino]benzoate obtained in Reference Example 15 322 mg (1.0 mmol), 4-phenyl-2-pyrrolidinone 177 mg (1.1 mmol), cesium carbonate 456 mg (1.4 mmol), tris(dibenzylideneacetone)dipalladium(0) 4.6 mg (0.005 mmol), Zandphos 8.7 mg (0.015 mmol) and 1,4-dioxane (2 mL) was stirred at 110° C. under argon atmosphere for 7 hours. The reaction solution was diluted with ethyl acetate and the resulting precipitates were filtered. The solvent was evaporated and the residual solid was purified by a column chromatography on silica gel (eluted with hexane/ethyl acetate=3:1→1:1) to give 329 mg (0.817 mmol) of the title compound (yield: 82%).

WORKUP

后处理

  1. customthe resulting precipitates
  2. filtrationwere filtered
  3. customThe solvent was evaporated
  4. customthe residual solid was purified by a column chromatography on silica gel (eluted with hexane/ethyl acetate=3:1→1:1)