HRID1892058

反应详情

EQUATION

反应方程式

HRID 1892058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2,3-dichloro-5-nitrobenzaldehyde (10 g, 0.045 mol) and methyl mercaptoacetate (6.6 mL, 0.06 mol) in DMF (200 mL) was added KOH (6 g) in 50 mL water. After stirring for 2 h, the reaction mixture was poured in ice cold water and the mixture was extracted in ethyl acetate. The organic layer was washed with water and dried. The evaporation of the solvent gave crude product which was purified by repetitive washing with hexane to yield 7-chloro-5-nitro-benzo[b]thiophene-2-carboxylic acid methyl ester, 12.3 g.

WORKUP

后处理

  1. additionthe reaction mixture was poured in ice cold water
  2. extractionthe mixture was extracted in ethyl acetate
  3. washThe organic layer was washed with water
  4. customdried
  5. customThe evaporation of the solvent
  6. customgave crude product which
  7. customwas purified
  8. washby repetitive washing with hexane