反应详情

A mixture of 250 mg of 1-[2-(2-carboxy-phenyl)-2-oxo-ethyl]-3-methyl-7-(3-methyl-2-buten-1-yl)-8-[3-(tert.-butyloxycarbonyl-amino)-piperidin-1-yl]-xanthine, 404 mg of ammonium carbonate, 135 mg of O-(benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium-tetrafluoroborate, 57 mg of hydroxybenzotriazole and 59 μl of triethylamine in 3 ml of tetrahydrofuran is stirred for eight hours at ambient temperature. For working up the reaction mixture is diluted with 30 ml of ethyl acetate and washed with 10% citric acid solution, 10% potassium carbonate solution and saturated sodium chloride solution. The organic phase is evaporated down and chromatographed through a silica gel column with methylene chloride/methanol (98:2 to 80:20).

1. washwashed with 10% citric acid solution, 10% potassium carbonate solution and saturated sodium chloride solution
2. customThe organic phase is evaporated down
3. customchromatographed through a silica gel column with methylene chloride/methanol (98:2 to 80:20)