反应详情

A mixture of 4.24 g of 3-chloro-2(R)-hydroxy-propyl-(cyclohexylmethyl)-phosphinic acid ethyl ester, 2.85 g of 1-(3,4-dichlorophenyl)ethylamine, 1.95 g of Hunig base and 15 ml of ethanol is heated at reflux for 4 days. After cooling to room temperature and removal of the solvent under reduced pressure, the reaction mixture is partitioned between dichloro-methane and water, dried over sodium sulfate and again concentrated to dryness by evaporation. Chromatography on silica gel yields 3-{N-[1-(3,4-dichlorophenyl)ethyl]amino}-2(S)-hydroxy-propyl(cyclohexylmethyl)phosphinic acid ethyl ester, [α]20D =-1.8°±0.9° (c=1.079 in chloroform).

1. temperatureis heated
2. temperatureat reflux for 4 days
3. customremoval of the solvent under reduced pressure
4. customthe reaction mixture is partitioned between dichloro-methane and water
5. dry with materialdried over sodium sulfate
6. concentrationagain concentrated to dryness by evaporation