反应详情

A mixture of 86 g of diethyl maleate, 144 g of butyraldehyde and 4 g of dibenzoyl peroxide was boiled at reflux for 20 hours. After completion of the reaction, the excess butyraldehyde was firstly distilled off over a Vigreux column and then the yellow coloured crude product was taken up in 250 ml of hexane and washed with 200 ml of 5% (wt./vol.) sodium hydrogen carbonate solution and 200 ml of water. The aqueous phases were back-extracted with a small amount of hexane. The combined organic phases were dried over sodium sulphate and freed from solvent on a rotary evaporator. Distillation of the resulting crude product in a high vacuum over a Vigreux column gave 104.5 g (85.6%) of diethyl 2-butyrylsuccinate as a slightly yellow coloured liquid; b.p. 84°-90° C./0.08 Torr.

1. temperatureat reflux for 20 hours
2. customAfter completion of the reaction
3. distillationthe excess butyraldehyde was firstly distilled off over a Vigreux column
4. washwashed with 200 ml of 5% (wt./vol.) sodium hydrogen carbonate solution and 200 ml of water
5. extractionThe aqueous phases were back-extracted with a small amount of hexane
6. dry with materialThe combined organic phases were dried over sodium sulphate
7. customfreed from solvent on a rotary evaporator
8. distillationDistillation of the resulting crude product in a high vacuum over a Vigreux column