反应详情

6-Amino-3-oxo-2,3-dihydro-indazole-1-carboxylic acid tert-butyl ester (69 mg, 0.277 mmol) and (5-Cyclopropyl-2H-pyrazol-3-yl)-(4,6-dichloro-[1,3,5]triazin-2-yl)-amine (50 mg, 0.184 mmol) were taken into 1 ml of n-butanol and stirred at room temperature for 2 hours. The solvent was evaporated in vacuo and the resulting white solid residue dissolved in dichloromethane-trifluoro acetic acid (1:1 mixture, 2 ml. After 3 hours, the solvent was evaporated in vacuo and the crude product purified by prep HPLC to afford 15 mg of the desired product as a white solid (16.4% yield). H-NMR(DMSO-d6, 500 mHz) δ 11.11(m, 1H), 10.41(s, 1H), 10.29(s, 1H), 7.11–7.82(m, 3H), 6.04(s, 1H), 1.84(m, 1H), 0.89(m, 2H), 0.60(m, 2H). MS (ES+): m/e=384.0 (M+H), 382.0 (M−H); LC/Method A/3.891 min, 98.0% purity by area %.

1. customThe solvent was evaporated in vacuo
2. dissolutionthe resulting white solid residue dissolved in dichloromethane-trifluoro acetic acid (1:1 mixture, 2 ml
3. waitAfter 3 hours
4. customthe solvent was evaporated in vacuo
5. customthe crude product purified by prep HPLC