HRID2109017

反应详情

EQUATION

反应方程式

HRID 2109017 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.36 g of trimethyloxonium tetrafluoroborate are added batchwise to a solution of 3.52 g of 1-acetyl-3-[1-hydroxy-1-(3-iodo-phenyl)-methylene]-6-chloro-2-indolinone (educt VII) and 2.72 ml of ethyldiisopropylamine in 80 ml dichloromethane and the mixture is stirred for one hour at ambient temperature. Then another 1.4 ml ethyldiisopropylamine and 1.2 g trimethyloxonium tetrafluoroborate are added and the mixture is stirred for a further two hours at ambient temperature. Then it is extracted with water, the organic phase is dried over magnesium sulphate and evaporated to dryness. The residue is recrystallised from ether and dried in vacuo at 80° C.

WORKUP

后处理

  1. stirringthe mixture is stirred for a further two hours at ambient temperature
  2. extractionThen it is extracted with water
  3. dry with materialthe organic phase is dried over magnesium sulphate
  4. customevaporated to dryness
  5. customThe residue is recrystallised from ether
  6. customdried in vacuo at 80° C.