dithiophosphoric acid o,o-diethyl ester; water;
reactants are commercially availlable.
general procedure: to a stirred solution of nitrile (36c?e, g and h) (4.58mmol) in h2o (0.92ml) were added dithiophosphoric acid o,o-diethyl ester (2.6ml, 16.5mmol), and the mixture was stirred at 80° c for 4h. after the reaction was quenched with saturated aqueous nahco3 (10ml), the organic phase wa s separated and the aqueous phase was extracted with diethylether (3?30ml). the combined organic pha ses were washed with brine (30ml), dried (mgso4), and concentrated in vacuo. the residue was purified by column chromatography (hexanes?etoac, 1:1) to give thioamide (34e?i).
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