反应详情

A mixture of 4-methyl-7-[methyl(2-thienylsulfonyl)amino]-1H-indole-2-carboxylic acid (2.2 g), 1H-1,2,3-benzotriazol-1-ol (1.2 g), N-[3-(dimethylamino)propyl]-N′-ethylcarbodiimide hydrochloride (1.5 g) and N,N-dimethylformamide (30 ml) was stirred at room temperature for 1 hr, and the mixture was further stirred at 60° C. for 1 hr. Then, 28% aqueous ammonia (2.0 mL) was added, and the mixture was stirred at room temperature for 3 hr. The reaction solution was concentrated under reduced pressure. The obtained residue was diluted with ethyl acetate, washed with water, aqueous sodium hydrogencarbonate solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained oil was crystallized from ethyl acetate-hexane to give the title compound (1.84 g, yield 84%) as colorless prism crystals. melting point 221-222° C.

1. stirringthe mixture was further stirred at 60° C. for 1 hr
2. stirringthe mixture was stirred at room temperature for 3 hr
3. concentrationThe reaction solution was concentrated under reduced pressure
4. additionThe obtained residue was diluted with ethyl acetate
5. washwashed with water, aqueous sodium hydrogencarbonate solution and saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe obtained oil was crystallized from ethyl acetate-hexane