反应详情

Ethyl 3-{5-[(hydroxyamino)(imino)methyl]-1H-indazol-1-yl}propanoate (D52) (265 mg, 0.96 mmol), 3-cyano-4-[(1-methylethyl)oxy]benzoic acid (can be prepared as described in WO2005/58848) (197 mg, 0.96 mmol), EDAC (203 mg) and HOBt (142 mg) were stirred in DMF (5 ml) at 80° C. for 2 hours. Stirred at room temperature over the weekend, then heated at 80° C. for a further 4 hours. The reaction mixture was cooled and then partitioned between EtOAc and sodium bicarbonate. The organic layer was separated, washed with brine, dried and evaporated to dryness in vacuo. The crude material was purified by flash chromatography to afford the title compound (214 mg) as a white solid. MS (ES): C24H23N5O4 requires 445; found (MH+) 446.

1. temperatureheated at 80° C. for a further 4 hours
2. temperatureThe reaction mixture was cooled
3. custompartitioned between EtOAc and sodium bicarbonate
4. customThe organic layer was separated
5. washwashed with brine
6. customdried
7. customevaporated to dryness in vacuo
8. customThe crude material was purified by flash chromatography