HRID732557

反应详情

EQUATION

反应方程式

HRID 732557 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Dissolve N-methyl-N-propyl-5-tributylstannanyl-isophthalamic acid methyl ester (885 mg, 168 mmol), 2-methyl-acryloyl chloride (172 mg, 1.64 mmol), tris(dibenzylideneacetone)dipalladium (46 mg, 0.05 mmol) and tricyclohexylphosphine (46 mg, 0.16 mmol)) in chloroform (15.5 mL) in a previously degassed vessel. Flush the mixture with nitrogen gas and heat the sealed mixture overnight at 60° C. Cool to room temperature and filter though a filtering agent. Concentrate the filtrate and purify (silica gel chromatography, eluting with 0:100 to 20:80 ethyl acetate:hexanes) to give the title compound.

WORKUP

后处理

  1. customFlush the mixture with nitrogen gas
  2. temperatureCool to room temperature
  3. filtrationfilter though a filtering agent
  4. concentrationConcentrate the filtrate
  5. custompurify
  6. wash(silica gel chromatography, eluting with 0:100 to 20:80 ethyl acetate:hexanes)