反应详情

A solution of ethyl (ethyl)(phenyl)phosphinate (130 mg, 0.66 mmol) in ethanol (0.5 ml) was treated with 4N HCl (1 ml) and refluxed for 22 hours. Tlc analysis revealed some residual starting material. The ethanol was removed on the rotary evaporator, an additional aliquot of 4N HCl (1 ml) was added, and reflux was resumed for a further six hours whereupon tlc analysis revealed complete consumption of starting material. The mixture was lyophillized to afford 110 mg (99%) of the title compound as a white solid; MS: 171 m/z (M+H)+ ; analysis calculated for C8H11O2P: C, 56.47; H, 6.53; P, 18.20; Found: C, 56.23; H, 6.35; P, 18.52.

1. temperaturerefluxed for 22 hours
2. customThe ethanol was removed on the rotary evaporator
3. additionan additional aliquot of 4N HCl (1 ml) was added
4. temperaturereflux
5. customconsumption of starting material