反応 #595342

反応方程式

hydrogen chloride

2,3-pentanedione 2-oxime

4-chlorobenzaldehyde

acetic acid

→

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

溶媒

diethyl ether

反応条件

後処理

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

実験手順

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.

出典