反应详情

温度

-50 °C

To a stirred, cold (-50° ) mixture of 7.00 g (0.0257 mole) of (2,4-difluoro-5-nitrophenyl) 1-pyrrolidinecarboxylate and 1.60 g (0.0283 mole) of methyl glycolate in 200 mL of tetrahydrofuran was added 1.02 g (0.0424 mole) of sodium hydride. The reaction mixture was stirred at -50° C. for approximately four hours. The mixture was allowed to gradually warm to room temperature. The reaction mixture was poured into ice-water, and the resultant mixture was extracted with diethyl ether. The extract was dried over anhydrous magnesium sulfate, filtered and the filtrate evaporated under reduced pressure to yield 4.5 g of (2-fluoro-4-methoxycarbonylmethoxy-5-nitrophenyl) 1-pyrrolidinecarboxylate. The nmr and ir spectra were consistent with the proposed structure.

1. temperatureto gradually warm to room temperature
2. extractionthe resultant mixture was extracted with diethyl ether
3. dry with materialThe extract was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. customthe filtrate evaporated under reduced pressure