HRID356836

反应详情

EQUATION

反应方程式

HRID 356836 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

105 g (0.48 mol) of 25 and 90 g (0.5 mol) of N-bromo-succinimide were dissolved in 2000 cm3 of tetrachloro-methane at room temperature, 3 g of azobisisobutyronitrile were added, and the mixture was refluxed for 4 hours. The succinimide which precipitated was filtered off, the solvent was removed in vacuo, and the residue was purified by filtration through 1000 g of silica gel (hexane/methylene chloride 9:1), giving 112 g (79%) of 26 as a colorless lachrymatory oil.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 4 hours
  2. customThe succinimide which precipitated
  3. filtrationwas filtered off
  4. customthe solvent was removed in vacuo
  5. filtrationthe residue was purified by filtration through 1000 g of silica gel (hexane/methylene chloride 9:1)