反应详情

温度

5 °C

In to a 5° C. solution of 4,5-dimethyl-2-(4-trifluoromethyl-phenyl)-oxazole N-oxide hydrochloride (113.71 g, 387.5 mmol) in CHCl3 (560 ml), was added phosphorus oxychloride (39.4 ml, 422.4 mmol) in CHCl3, dropwise over 15 min. The reaction was refluxed for 2.5 h, then cooled to 5° C., poured into ice water, and basified with NaOH (1N). The organic layer was dried over MgSO4. Evaporation and recrystallization from ether/hexane, gave a yellow solid (30.0 g, 28% yield, mp 84°-85° C.).

1. temperatureThe reaction was refluxed for 2.5 h
2. dry with materialThe organic layer was dried over MgSO4
3. customEvaporation and recrystallization from ether/hexane