HRID1196173

反应详情

EQUATION

反应方程式

HRID 1196173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dehydrolinalool (60.8 g, 0.4 mol), bromoform (151.6 g, 0.6 mol) and 0.8 g of triethylbenzylammonium chloride are placed in a reaction flask and 64 g of a 50% sodium hydroxide solution are added during 30 minutes. The reaction is exothermic and the mixture is therefore cooled with ice. After stirring the mixture at room temperature for 21.5 hours the same amounts of bromoform and triethylbenzylammonium chloride are again added. The reaction becomes exothermic and is cooled with ice. The mixture is left to react at 0° for a further 4 hours, poured onto ice and extracted with methylene chloride. The organic phases are washed neutral, dried and evaporated. In this manner there are obtained 109.5 g (84%) of 5-(2'2'-dibromo-3'3'-dimethylcyclopropyl)-3-methyl-1-pentyn-3-ol.

WORKUP

后处理

  1. temperaturethe mixture is therefore cooled with ice
  2. additionare again added
  3. temperatureis cooled with ice
  4. waitThe mixture is left
  5. customto react at 0° for a further 4 hours
  6. additionpoured onto ice
  7. extractionextracted with methylene chloride
  8. washThe organic phases are washed neutral
  9. customdried
  10. customevaporated