反应详情

温度

80 °C

Successively, sulfuric acid 62% (79.4 g, 0.5 mol), aqueous formaldehyde 35% (82 g, 1.0 mol) and cyclohexyl acetaldehyde (100.8 g, 0.8 mol) were added slowly to diethylamine (73 g, 1.0 mol) at 0° C. After stirring at 80° C. overnight, the reaction mixture was extracted with MTBE. The combined organic phases were washed with H2O until neutral pH was achieved, dried (MgSO4) and concentrated in vacuo. The crude product was distilled under reduced pressure using a Widmer column (10 Torr, 80° C.) yielding 89.5 g (81%) of pure product as colorless oil.

1. extractionthe reaction mixture was extracted with MTBE
2. washThe combined organic phases were washed with H2O until neutral pH
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. distillationThe crude product was distilled under reduced pressure
6. customa Widmer column (10 Torr, 80° C.)