반응 #595342

반응 방정식

hydrogen chloride

2,3-pentanedione 2-oxime

4-chlorobenzaldehyde

acetic acid

→

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

용매

diethyl ether

반응 조건

후처리

1. 1
   workup.ADDITIONis then introduced for 30 min
2. 2
   기타A precipitate is formed
3. 3
   여과which is filtered off with suction
4. 4
   세척washed twice with in each case 2 ml of diethyl ether
5. 5
   추출The suspension is then extracted four times with in each case 10 ml of dichloromethane
6. 6
   건조The combined organic phases are dried over magnesium sulfate
7. 7
   기타the solvent is removed on a rotary evaporator
8. 8
   기타The residue is used without further purification in the subsequent reaction

실험 절차

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.

출처