HRID356833
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
114 g (0.52 mol) of 18 and 103 g (0.58 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 141 g (82%) of 19 as a colorless lachrymatory oil.
WORKUP
后处理
- temperaturethe mixture was refluxed for 4 hours
- customThe succinimide which precipitated
- filtrationwas filtered off
- customthe solvent was removed in vacuo
- filtrationthe residue was purified by filtration through 1000 g of silica gel (hexane/methylene chloride 9:1)