Methanesulfonic Acid → HCID 57153572, compound

Participants

Reaction Steps

To a solution of the compound (373 mg) obtained in the above (1) in acetonitrile (1.5 ml) is added dropwise a solution of methanesulfonic acid (380 mg) in acetonitrile (1.5 ml), and the mixture is stirred at room temperature for 30 minutes. To the mixture are added dropwise DMF (4 ml) and triethylamine (400 mg) at 5°-10° C. under ice-cooling, and further thereto am added 4-cyanobenzoic acid (129 mg), HOBT.H2O (146 mg) and then further WSC.HCl (183 mg). The mixture is stirred at 5°-10° C. for 30 minutes, and further stirred at room temperature for 12 hours. The reaction mixture is poured into water, and extracted with ethyl acetate. The combined organic layers are washed successively with 1N hydrochloric acid, a saturated aqueous sodium hydrogen carbonate solution and a saturated brine (each twice), and dried over magnesium sulfate. The desiccant is removed by filtration, and the filtrate is concentrated under reduced pressure to give the title compound (390 mg) as a white powder.

Provenance & Evidence