反应详情

温度

80 °C

The title compound was prepared by reacting 3-bromo-1-perhydro-2H-pyran-2-yl-1H-indazole-5-carboxamide (15.13 g, 46.67 mmol) with N,N-dimethylformamide dimethyl acetal (134 mL) and heating to 80° C. for 3 hours. The reaction was allowed to cool to room temperature, and condensed to a brown oil that was exposed to atmospheric conditions minimally. To the crude oil was added glacial acetic acid (220 mL) and hydrazine (23 mL), and then the mixture was heated to 115° C. for 1.5 hours. The reaction was allowed to cool to room temperature, and subsequently added to water (500 mL) resulting in the formation of a white precipitate which was filtered and dried in a vacuum oven (15.05 g, 93% yield): ES-MS (m/z) 350 [M+1]+.

1. temperatureto cool to room temperature
2. customcondensed to a brown oil that
3. temperaturethe mixture was heated to 115° C. for 1.5 hours
4. temperatureto cool to room temperature
5. customresulting in the formation of a white precipitate which
6. filtrationwas filtered
7. customdried in a vacuum oven (15.05 g, 93% yield)