反应详情

温度

100 °C

To a 50 mL flask charged with DMF (5 mL) was added POCl3 (0.7 g, 4.6 mmol) dropwise at 0° C. After stirring for 10 min, a solution of 2-phenyloxazole (0.6 g, 4.1 mmol) in DMF (5 mL) was added dropwise. The reaction mixture was heated to 100° C. and stirred for 48 h. After cooling to room temperature, the reaction mixture was poured into ice water and the pH was adjusted to 10 with 10% aqueous NaOH. The aqueous mixture was extracted with EtOAc (20 mL×3). The combined organic layers were dried over Na2SO4 and filtered. The filtrate was concentrated and purified by column chromatography to give 240 mg of the desired product. LC-MS: m/z 174 (M+H+).

1. stirringstirred for 48 h
2. temperatureAfter cooling to room temperature
3. extractionThe aqueous mixture was extracted with EtOAc (20 mL×3)
4. dry with materialThe combined organic layers were dried over Na2SO4
5. filtrationfiltered
6. concentrationThe filtrate was concentrated
7. custompurified by column chromatography