HRID1446812
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewhile cooling
- temperaturethe mixture heated to 68° for 4 hours
- customat about 30°
- customThe precipitate formed
- filtrationis filtered off
- washwashed with 16 lt of toluene
- customThe filtrate is separated
- washthe organic layer washed 3 times with 27 lt of water
- customevaporated
- distillationthe residue distilled
- customthe fraction boiling at 170°/0.2 mmHg collected