反应详情

30.0 mL Benzaldehyde was dissolved in 150 mL EtOH and cooled with an ice bath. Added was 5.01 mL 45% KOH (0.2 equiv.), followed by dropwise addition of 16.5 mL butyraldehyde. The mixture was stirred for 3 days at room temperature, acidified with 1M HCl and extracted with ether. The organic layer was dried over Na2SO4, filtrated and concentrated in vacuo. Vacuum distillation yielded 20.4 g of a yellow fluid (78-82° C., 0.6 mbar) containing 70% of the desired product. This material was used in subsequent steps without further purification. Characteristic signals in 1H NMR (400 MHz, CDCl3): δ 1.15 (t, J=7.5 Hz, 3H), 2.57 (q, J=7.5 Hz, 1H), 7.22 (s, 1H), 9.56 (s, 1H).

1. temperaturecooled with an ice bath
2. additionAdded
3. extractionextracted with ether
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltrated
6. concentrationconcentrated in vacuo
7. distillationVacuum distillation
8. customyielded 20.4 g of a yellow fluid (78-82° C., 0.6 mbar)