反应详情

温度

80 °C

3-Cyano-4-[(1-methylethyl)oxy]benzoic acid (can be prepared as described in WO2005/58848) (1.52 g), EDAC (2.14 g) and HOBt (1.51 g) were dissolved in DMF (30 ml) and then stirred for 5 minutes. N-hydroxy-1H-indazole-5-carboximidamide (D2) (1.3 g) was added and the reaction was heated to 80° C. for 6 hours and left to cool overnight. The solvent was removed in vacuo and the crude was partitioned between EtOAc and aq. sodium bicarbonate. The organic layer was separated, dried and evaporated to dryness in vacuo. The resulting solid was triturated with ether and ethyl acetate, washed with methanol and ether to give the title compound (816 mg) as a pink solid. MS (ES): C19H15N5O2 requires 345; found (MH+) 346

1. waitleft
2. temperatureto cool overnight
3. customThe solvent was removed in vacuo
4. customthe crude was partitioned between EtOAc and aq. sodium bicarbonate
5. customThe organic layer was separated
6. customdried
7. customevaporated to dryness in vacuo
8. customThe resulting solid was triturated with ether and ethyl acetate
9. washwashed with methanol and ether