HRID1421183

反应详情

EQUATION

反应方程式

HRID 1421183 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.57 ml of oxalyl chloride were added to a solution of 5.7 g of 1-(2-acetoxyethyl)indole in 70 ml of dichloromethane at 0° C. The resulting solution was stirred for 2 hours and the solvent was then evaporated. To the residue, dissolved in 210 ml of dichloromethane, were added 7.7 ml of triethylamine and 5.29 g of 1-methylindole-3-acetic acid under a nitrogen atmosphere. After stirring for 18 hours the solvent was evaporated and the residue was purified on silica gel with ethyl acetate/petroleum ether (1:2). Crystallization from ethyl acetate/hexane gave 1.87 g of 3-[1-(2-acetoxyethyl)-3-indolyl]-4-(1-methyl-3-indolyl)furan-2,5-dione, m.p. 198°-199° C.

WORKUP

后处理

  1. customthe solvent was then evaporated
  2. dissolutionTo the residue, dissolved in 210 ml of dichloromethane
  3. additionwere added 7.7 ml of triethylamine and 5.29 g of 1-methylindole-3-acetic acid under a nitrogen atmosphere
  4. stirringAfter stirring for 18 hours the solvent
  5. customwas evaporated
  6. customthe residue was purified on silica gel with ethyl acetate/petroleum ether (1:2)
  7. customCrystallization from ethyl acetate/hexane