HRID1443456

反应详情

EQUATION

反应方程式

HRID 1443456 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Fluoro benzoic acid (700 mg, 5 mmol) was dissolved in dichloromethane (20 ml) and pyridine (2 ml). 2-Amino-4-methoxy-3-methyl-benzoic acid methyl ester (81) (878 mg, 4.5 mmol) was added and the mixture was refluxed for 5 h. Water was added and the mixture was extracted with dichloromethane. The organic phase was dried, filtered and evaporated and the afforded residue was purified by column chromatography on silica gel, eluted with ether-pentane 1:1 which gave pure title compound (870 mg, 61%). MS (M+H+) 318.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 5 h
  2. extractionthe mixture was extracted with dichloromethane
  3. customThe organic phase was dried
  4. filtrationfiltered
  5. customevaporated
  6. customthe afforded residue was purified by column chromatography on silica gel
  7. washeluted with ether-pentane 1:1 which