反应详情

A solution of 38.3 g of ethyl P-cyclohexylmethyl-P-diethoxymethylphosphinate in 27 ml of water is treated with 27 ml of 37% aqueous hydrochloric acid and the mixture heated to reflux for 5 hours. The mixture is cooled to room temperature and washed with ether/hexane 1:1. Three phases are obtained. The lower 2 phases are removed and the water is removed under reduced pressure to afford cyclohexylmethylphosphonous acid as a white solid; 1H-NMR (CDCl3): δ (ppm)=7.40 (1H, broad singlet, exchanges D2O, P--OH), 7.12 (1H, d, J=526 Hz, H--P), 2.10-1.75 (7H, m, 3×CH2 +CH), 1.48-1.05 (6H, m, 3×CH3).

1. temperaturethe mixture heated
2. temperatureto reflux for 5 hours
3. washwashed with ether/hexane 1:1
4. customThree phases are obtained
5. customThe lower 2 phases are removed
6. customthe water is removed under reduced pressure