反应详情

温度

75 °C

A mixture of N-(cyclopropylmethyl)-2-(3-iodo-4-methylpyridin-2-yl)hydrazinecarboxamide (preparation 28c, 0.85 g, 2.5 mmol) and phosphorous oxychloride (10 mL) was stirred at 75° C. overnight. The reaction mixture was cooled to ambient temperature and added slowly to an ice-water mixture and then ethyl acetate was added. To the cooled, stirred, biphasic mixture was added aqueous sodium hydroxide solution until the aqueous layer reached a pH of 8. The organic layer was washed with water, brine, dried (MgSO4) and the solvent evaporated in vacuo to yield the title compound (0.77 g, 96%) as a pale yellow solid.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. stirringTo the cooled, stirred
3. washThe organic layer was washed with water, brine
4. dry with materialdried (MgSO4)
5. customthe solvent evaporated in vacuo