Diethyl cyanophosphonate → HCID 21993780, compound

Participants

Reaction Steps

To a solution of 0.406 g (1.860 mM) of 5-thia-1,8b-diazaacenaphthylene-4-carboxylic acid, 0.62 g (2.05 mM) of 1-(3-phenylpropan-1-yl)piperidin-3-ylmethylamine dihydrochloride, and 1.04 ml (7.44 mM) of triethylamine in 10 ml of N,N-dimethylformamide was added 0.34 ml (2.23 mM) of diethyl cyanophosphate at room temperature and the mixture was stirred at the prevailing temperature overnight. This reaction mixture was poured in aqueous solution of sodium hydrogen carbonate and extracted with 3 portions of ethyl acetate. The organic layers were pooled and dried over MgSO4 and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate to ethyl acetate-methanol=4/1 to 2/1) to provide the title compound.

Provenance & Evidence