HRID2304875

反应详情

EQUATION

反应方程式

HRID 2304875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. customAt the time when about 1 hour and 30 minutes
  4. customThe suspension obtained
  5. temperatureto cool
  6. temperaturewas cooled on ice
  7. filtrationthe precipitated crystal was recovered by a filtration
  8. washwashed with cool ethyl acetate and water