HRID1659890

反应详情

EQUATION

反应方程式

HRID 1659890 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.44 g of 55% strength sodium hydride in paraffin oil (0.15 mole) are introduced into 200 ml of absolute dimethylsulfoxide and 30 g (0.15 mole) of 3-methyl-5-(2-hydroxy-styryl)-isoxazole, dissolved in 50 ml of dimethylsulfoxide, are added dropwise, at room temperature. When the evolution of hydrogen has ceased, 20.2 g (0.15 mole) of epibromohydrin are added dropwise and the reaction mixture is stirred for 20 hours at room temperature. It is then poured onto 1.5 liters of ice water and the solid residue is filtered off and recrystallized from isopropanol. 26.2 g (68% of theory) of colorless crystals, of melting point 99°-100° C., are obtained.

WORKUP

后处理

  1. additionare added dropwise, at room temperature
  2. filtrationthe solid residue is filtered off
  3. customrecrystallized from isopropanol
  4. custom26.2 g (68% of theory) of colorless crystals, of melting point 99°-100° C., are obtained