HRID1702216

反应详情

EQUATION

反应方程式

HRID 1702216 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To 130 lt of ethanol, 12.1 kg of sodium methoxide are added while cooling and stirring, followed by 26.5 kg of salicylaldehyde at 30°. Thereupon 33.3 kg of trans-1,4-dichloro-2-butene are added and the mixture heated to 68° for 4 hours. It is combined with 156 lt of toluene, 187 lt of water and 9.4 kg of 36% hydrochloric acid while keeping the temperature at about 30°. The precipitate formed is filtered off and washed with 16 lt of toluene. The filtrate is separated, the organic layer washed 3 times with 27 lt of water, evaporated, the residue distilled and the fraction boiling at 170°/0.2 mmHg collected, to yield the 2-(4-chloro-trans-2-butenyloxy)benzaldehyde.

WORKUP

后处理

  1. temperaturewhile cooling
  2. temperaturethe mixture heated to 68° for 4 hours
  3. customat about 30°
  4. customThe precipitate formed
  5. filtrationis filtered off
  6. washwashed with 16 lt of toluene
  7. customThe filtrate is separated
  8. washthe organic layer washed 3 times with 27 lt of water
  9. customevaporated
  10. distillationthe residue distilled
  11. customthe fraction boiling at 170°/0.2 mmHg collected