HRID981262

反应详情

EQUATION

反应方程式

HRID 981262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 30 ml of diethyl ether was dissolved 3.08 g of ethyl 4-(1-diphenylmethoxycarbonylvinyl)-2,3,5-trifluorobenzoate. To the resulting solution was added, with ice-cooling, a diazomethane-diethyl ether solution prepared from 2.00 g of N-methyl-N-nitrosourea. The resulting mixture was stirred at room temperature for 12 hours. The reaction mixture was concentrated under reduced pressure. The residue obtained was dissolved in 30 ml of toluene. The resulting solution was stirred at 60° C. for 1 hour. The reaction mixture was concentrated under reduced pressure. The residue obtained was purified by a column chromatography (eluant: toluene) to obtain 2.90 g (yield: 91.2%) of ethyl 4-(1-diphenylmethoxycarbonyl-2-methylvinyl)-2,3,5-trifluorobenzoate.

WORKUP

后处理

  1. additionTo the resulting solution was added, with ice-
  2. temperaturecooling
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customThe residue obtained
  5. stirringThe resulting solution was stirred at 60° C. for 1 hour
  6. concentrationThe reaction mixture was concentrated under reduced pressure
  7. customThe residue obtained
  8. customwas purified by a column chromatography (eluant: toluene)