HRID2304875
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
The compound obtained in Example 15 (1.8 g) was admixed with N-bromosuccinimide (0.88 g), azobisisobutyronitrile (70 mg) and ethyl acetate (18 ml) and the mixture was heated under reflux for 2 hours. At the time when about 1 hour and 30 minutes had elapsed during this procedure, the suspension turned into a solution. The suspension obtained after allowing to cool was cooled on ice, and the precipitated crystal was recovered by a filtration, washed with cool ethyl acetate and water to obtain the title compound (1.68 g, 79.1%).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 2 hours
- customAt the time when about 1 hour and 30 minutes
- customThe suspension obtained
- temperatureto cool
- temperaturewas cooled on ice
- filtrationthe precipitated crystal was recovered by a filtration
- washwashed with cool ethyl acetate and water