反应详情

温度

0 °C

A solution of methyl 1-methyl-1H-indazole-6-carboxylate (230 mg, 1.21 mmol, PREPARATION 4) in anhydrous THF (4 mL) was cooled to 0° C., LiAlH4 (92 mg, 2.42 mmol) was added in portions below 0° C., and the mixture was then stirred at 0° C. for 1.5 h, added water:10% NaOH: water=0.2 mL: 0.2 mL: 0.6 mL carefully, filtered, and the filtrate was concentrated and purified by silica gel flash column to give 192 mg of crude product which was used directly for next step (98%). [M+H] Calc'd for C9H10N2O, 163; Found, 163.

1. filtration10% NaOH: water=0.2 mL: 0.2 mL: 0.6 mL carefully, filtered
2. concentrationthe filtrate was concentrated
3. custompurified by silica gel flash column