HRID1108709

反应详情

EQUATION

反应方程式

HRID 1108709 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of methyl 2-propylindole-6-carboxylate (10 g), methoxyacetic acid (4.6 ml) and carbontetrachloride (13.4 ml) in 1,2-dichloroethane (45 ml) was added slowly triphenylphosphine (16.7 g) in 1,2-dichloroethane (30 ml) over 1 hour under reflux, and the resulting mixture was heated under reflux for additional 8 hours. After evaporation of solvent, the residue was chromatographed on silica gel eluting with a mixture of hexane and ethyl acetate (1:1) and triturated with diethyl ether to give methyl 3-methoxyacetyl-2-propylindole-6-carboxylate (8.11 g).

WORKUP

后处理

  1. temperatureunder reflux
  2. temperaturethe resulting mixture was heated
  3. temperatureunder reflux for additional 8 hours
  4. customAfter evaporation of solvent
  5. customthe residue was chromatographed on silica gel eluting with a mixture of hexane and ethyl acetate (1:1)
  6. customtriturated with diethyl ether