反应详情

A solution of 38 bg of ethyl diethoxymethyl(benzyl)phosphinate in 300 ml of absolute ethanol is treated with 20 g of Raney nickel and the suspension is hydrogenated at 110° C. and 150 bar for 12 hours. After this time the mixture is filtered through celite® and the filtrate is evaporated to dryness. Distillation of the residue in high vacuum gives ethyl diethoxymethyl(cyclohexylmethyl)phosphinate of b.p. 120° (10-2 mbar). 1H-NMR (CDCl3): δ (ppm)=, 4.62 (1H, d, CHP), 4.17 (2H, m, CH2OP), 3.84+3.69 (2H, m, 2×CH2OC), 1.88 (3H, m, CH2P+CH), 1.68 (6H, m, 3×CH2), 1.30 (13H, m, 3×CH3 +2×CH2).

1. customis hydrogenated at 110° C.
2. filtrationAfter this time the mixture is filtered through celite®
3. customthe filtrate is evaporated to dryness
4. distillationDistillation of the residue in high vacuum