反应 #595342

反应方程式

hydrogen chloride

2,3-pentanedione 2-oxime

4-chlorobenzaldehyde

acetic acid

→

2-(4-Chlorophenyl)-5-ethyl-4-methyl-1,3-oxazole 3-oxide

溶剂

diethyl ether

反应条件

后处理

1. 1
   workup.ADDITIONis then introduced for 30 min
2. 2
   其他A precipitate is formed
3. 3
   过滤which is filtered off with suction
4. 4
   洗涤washed twice with in each case 2 ml of diethyl ether
5. 5
   萃取The suspension is then extracted four times with in each case 10 ml of dichloromethane
6. 6
   干燥The combined organic phases are dried over magnesium sulfate
7. 7
   其他the solvent is removed on a rotary evaporator
8. 8
   其他The residue is used without further purification in the subsequent reaction

实验过程

1.00 g (8.69 mmol) of 2,3-pentanedione 2-oxime and 1.34 g (9.55 mmol) of 4-chlorobenzaldehyde are initially charged in 2 ml (34.94 mmol) of glacial acetic acid. With ice-cooling of the reaction mixture, hydrogen chloride gas is then introduced for 30 min. 10 ml of diethyl ether are then added to the reaction mixture. A precipitate is formed, which is filtered off with suction and washed twice with in each case 2 ml of diethyl ether. The precipitate is resuspended in about 5 ml of water, and the suspension is made basic using ammonia. The suspension is then extracted four times with in each case 10 ml of dichloromethane. The combined organic phases are dried over magnesium sulfate and the solvent is removed on a rotary evaporator. The residue is used without further purification in the subsequent reaction.

来源