反应详情

To a suspension of sodium hydride (60% dispersion in oil, 2.2 g, 55 mmol) in tetrahydrofuran (100 ml) at 0° C. was added ethyl 2-(diethoxyphosphoryl)acetate (11.2 g, 50 mmol) over 30 min, and the mixture was stirred at room temperature for 1 h. To this was added 4,4-dimethyl-2-cyclohexene-1-one over 20 min and the reaction mixture was stirred for a further 1 h. Water (100 ml) was added and the mixture was extracted with ether (2×100 ml). The combined extracts were dried (MgSO4), filtered and concentrated in vacuo to afford the title compound as a colourless oil (9.7 g, 100%).

1. stirringthe reaction mixture was stirred for a further 1 h
2. extractionthe mixture was extracted with ether (2×100 ml)
3. dry with materialThe combined extracts were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo