HRID359310

反应详情

EQUATION

反应方程式

HRID 359310 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

50 g (0.328 mol) of d-camphor are dissolved in 400 cm3 of 1,2-dimethoxyethane. 17.5 g of sodium hydride (0.73 mol) are added and the mixture is brought to reflux for one hour. 70 g (0.3 mol) of 3,5-di-tert-butyl-4-hydroxybenzaldehyde are added and the mixture is heated under reflux for 10 hours. After being cooled, the reaction medium is gradually diluted with 100 cm3 of ethanol and then with 100 cm3 of water. The mixture is acidified by adding 10% strength hydrochloric acid. The precipitate formed is filtered off, washed with water and dried. After recrystallization in isopropyl ether and then in ethanol, 54.5 g (49% yield) of expected product are obtained, possessing the following characteristics:

WORKUP

后处理

  1. temperatureto reflux for one hour
  2. temperaturethe mixture is heated
  3. temperatureunder reflux for 10 hours
  4. temperatureAfter being cooled
  5. customThe precipitate formed
  6. filtrationis filtered off
  7. washwashed with water
  8. customdried
  9. customAfter recrystallization in isopropyl ether