反应详情

250 mg (0.86 mmol) of 3-[1-(3-aminophenyl)ethyl]-5,6-difluoro-3H-benzoxazol-2-one, 137 mg (0.95 mmol) of 2-(4-methylpiperazin-1-yl)ethanol and 200 μl (1.81 mmol) of N-methylmorpholine are suspended in 10 ml of dichloromethane, the mixture is stirred at room temperature for 10 min, and 128 mg (0.43 mmol) of bis(trichloromethyl) carbonate are added. The reaction mixture is stirred at room temperature for 16 h. The mixture is subsequently diluted with 30 ml of dichloromethane, washed with 2×20 ml of saturated sodium hydrogencarbonate solution, dried over sodium sulfate and evaporated to dryness. The crude product is purified by column chromatography on silica gel, dissolved in acetone, warmed with HCl in ether and, when crystallisation is complete, filtered off with suction and dried. Product (“A27”): 95 mg, product is in the form of the hydrochloride;

1. stirringThe reaction mixture is stirred at room temperature for 16 h
2. washwashed with 2×20 ml of saturated sodium hydrogencarbonate solution
3. dry with materialdried over sodium sulfate
4. customevaporated to dryness
5. customThe crude product is purified by column chromatography on silica gel
6. dissolutiondissolved in acetone
7. temperaturewarmed with HCl in ether and, when crystallisation
8. filtrationfiltered off with suction
9. customdried