反应详情

温度

0 °C

To a stirred solution of diisopropylamine (13.0 g) in tetrahydrofurane (160 mL) was added a solution of n-butyllithium in hexane (51.4 mL; c=2.5 M) at −78° C. The solution was stirred at 0° C. for 15 minutes. The solution was cooled to −78° C. and a solution of methyl (4-fluorophenyl)acetate (18.0 g), dissolved in tetrahydrofurane (40 mL) was added. The solution was stirred at −78° C. for 30 minutes. Methyl iodide (10.0 mL) was added at −78° C., and the solution was allowed to warm up to 0° C. within 1 h. Water was added and the reaction mixture was extracted with ethyl acetate. The organic phase was dried (sodium sulfate) and the solvent was removed in vacuum. Silicagel chromatography gave 18.9 g of the title compound.

1. temperatureThe solution was cooled to −78° C.
2. additionwas added
3. stirringThe solution was stirred at −78° C. for 30 minutes
4. temperatureto warm up to 0° C. within 1 h
5. extractionthe reaction mixture was extracted with ethyl acetate
6. dry with materialThe organic phase was dried (sodium sulfate)
7. customthe solvent was removed in vacuum