HRID506873

反应详情

EQUATION

反应方程式

HRID 506873 的结构方程式

PROCEDURE

实验过程

To AlCl3 (9.9 g, 75 mmol) is added dropwise 6-acetyltetralin (5.25 g, 30 mmol) under mechanical stirring at RT. After 20 minutes at 70° C. the reaction is cooled to RT and treated in small portions with Br2 (5.76 g [=1.86 ml], 36 mmol) over a period of 30 minutes. After that the mixture is stirred for further 60 minutes at 85° C. After cooling down to RT and addition of ice-water (450 ml) the compound is extracted with methylene chloride and purified on silica gel using a mixture of cyclo-hexane/ethyl acetate 2/1 to 1/1 obtaining the product as a pale yellow solid.

WORKUP

后处理

  1. temperatureAfter 20 minutes at 70° C. the reaction is cooled to RT
  2. stirringAfter that the mixture is stirred for further 60 minutes at 85° C
  3. temperatureAfter cooling down to RT
  4. extractionis extracted with methylene chloride
  5. custompurified on silica gel using
  6. additiona mixture of cyclo-hexane/ethyl acetate 2/1 to 1/1 obtaining the product as a pale yellow solid