反应详情

温度

115 °C

A mixture of tert-butyl 4-hydroxyphenethylcarbamate (700 g, 2.94 mmol), 2,2-difluoropropyl methanesulfonate (668 mg, 3.84 mmol) and cesium carbonate (1.92 g, 5.88 mmol) in DMF (5 mL) was stirred at 115° C. in a microwave reactor for 3 h. After cooling to room temperature, water was added and extracted with ethyl acetate (3×100 mL). The combined organic layers were washed with brine, dried over anhydrous sodium sulfate and filtered. The filtrate was evaporated under vacuum to give the crude product, which was purified by preparative thin layer chromatography (22% ethyl acetate in petroleum ether) to afford the title compound (130 mg, 0.41 mmol, 14% yield). MS (ESI) m/z 316.1 [M+H]+.

1. temperatureAfter cooling to room temperature
2. extractionextracted with ethyl acetate (3×100 mL)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. customThe filtrate was evaporated under vacuum
7. customto give the crude product, which
8. customwas purified by preparative thin layer chromatography (22% ethyl acetate in petroleum ether)