反应详情

To a suspension of N-(thiazolo[4,5-c]pyridin-2-yl)acetamide, prepared in the previous step, in MeOH (200 mL) at room temperature was added lithium hydroxide hydrate (7.08 g, 169 mmol). The reaction mixture was stirred at room temperature for 30 min and then warmed to 40° C. After 3 h, additional lithium hydroxide hydrate (7.48 g) was added. The reaction mixture was heated to 50° C. for 20 h and concentrated. The reaction mixture was diluted with DCM/MeOH (˜10:1, 500 mL). The undissolved material was removed by filtration and the filtrate was concentrated. Purification by flash column chromatography on silica gel (eluted with 2% to 10% MeOH in DCM) gave thiazolo[4,5-c]pyridin-2-amine.

1. temperaturewarmed to 40° C
2. waitAfter 3 h
3. temperatureThe reaction mixture was heated to 50° C. for 20 h
4. concentrationconcentrated
5. additionThe reaction mixture was diluted with DCM/MeOH (˜10:1, 500 mL)
6. customThe undissolved material was removed by filtration
7. concentrationthe filtrate was concentrated
8. customPurification by flash column chromatography on silica gel (eluted with 2% to 10% MeOH in DCM)