HRID732552

反应详情

EQUATION

反应方程式

HRID 732552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Dissolve N-methyl-N-propyl-5-tributylstannanyl-isophthalamic acid methyl ester (500 mg, 1 mmol), furan-2-carbonyl chloride (0.12 mL), tris(dibenzylideneacetone)-dipalladium (0) (19 mg) and 2-(di-tert-butylphosphino)biphenyl (35 mg) in THF (6 mL) in a previously degassed, sealed vessel. Flush the mixture with nitrogen and heat the sealed mixture overnight at 50° C. Cool the reaction to room temperature and filter though a filtering agent. Concentrate the filtrate and purify (silica gel chromatography, 0:100 to 38:62 ethyl acetate:hexanes) to give the title compound (50%).

WORKUP

后处理

  1. customa previously degassed
  2. customsealed vessel
  3. customFlush the mixture with nitrogen
  4. temperatureCool
  5. customthe reaction to room temperature
  6. filtrationfilter though a filtering agent
  7. concentrationConcentrate the filtrate
  8. custompurify (silica gel chromatography, 0:100 to 38:62 ethyl acetate:hexanes)