HRID1089356

反应详情

EQUATION

反应方程式

HRID 1089356 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10 g of 4-acetoxy-3,5-dibromostyrene are dissolved in 50 ml THF and 25 ml methanol, 12 g hydrazine hydrate (80% aqueous solution) is added, and the cloudy mixture is then converted into a clear solution by adding 3 ml of water. After 40 minutes it is acidified with a semi-concentrated HCl to pH 2 and extracted twice with ether, the ether phase is washed twice with water and dried over sodium sulfate, and the ether is removed with a rotary evaporator at room temperature under aspirator vacuum. 8.5 g of crude product remain, from which 6.45 g of white crystals (mp 74° C.) are obtained by recrystallization from petroleum ether.

WORKUP

后处理

  1. extractionextracted twice with ether
  2. washthe ether phase is washed twice with water
  3. dry with materialdried over sodium sulfate
  4. customthe ether is removed with a rotary evaporator at room temperature under aspirator vacuum
  5. customare obtained by recrystallization from petroleum ether