Реакция #595342

Уравнение реакции

hydrogen chloride

2,3-pentanedione 2-oxime

4-chlorobenzaldehyde

acetic acid

→

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

Растворители

diethyl ether

Условия реакции

Обработка

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

Методика

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.

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