反应详情

To a mixture of 2-(tritylthio)ethylamine hydrochloride (0.93 g), triethylamine (0.37 mL) and N,N-dimethylformamide (15 mL) were added 4-methyl-7-[(2-thienylsulfonyl)amino]-1H-indole-2-carboxylic acid (0.73 g), 1H-1,2,3-benzotriazol-1-ol (0.47 g) and N-[3-(dimethylamino)propyl]-N′-ethylcarbodiimide hydrochloride (0.59 g) under ice-cooling, and the mixture was stirred at room temperature for 15 hr. The reaction mixture was diluted with ethyl acetate, washed with aqueous citric acid solution, aqueous sodium hydrogencarbonate solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained crystals were washed with ethyl acetate-hexane to give the title compound (1.31 g, yield 95%) as pale-yellow crystals. melting point 241-242° C.

1. temperaturecooling
2. washwashed with aqueous citric acid solution, aqueous sodium hydrogencarbonate solution and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. washThe obtained crystals were washed with ethyl acetate-hexane