反应详情

1.00 g (9.89 mmol) of diacetyl monoxime and 1.53 g (10.88 mmol) of 4-chlorobenzaldehyde are initially charged in 2 ml (34.94 mmol) of glacial acetic acid. With ice-cooling, hydrogen chloride gas is then introduced into the reaction mixture 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 suspended in about 5 ml of water, and the suspension is made basic using aqueous ammonia. The suspension is then extracted four times with in each case 10 ml of dichloromethane. The combined organic phases are dried over magnesium sulphate, and the solvent is removed on a rotary evaporator. Without further purification, the product obtained in this manner is used for the subsequent step.

1. temperatureWith ice-cooling
2. additionare then added to the reaction mixture
3. customA precipitate is formed
4. filtrationwhich is filtered off with suction
5. washwashed twice with in each case 2 ml of diethyl ether
6. extractionThe suspension is then extracted four times with in each case 10 ml of dichloromethane
7. dry with materialThe combined organic phases are dried over magnesium sulphate
8. customthe solvent is removed on a rotary evaporator
9. customWithout further purification
10. customthe product obtained in this manner