反应详情

温度

90 °C

A mixture of (2S,3S)-3-(1-hydroxy-1-methylethyl)-2-methylpyrrolidine 1/2 oxalate (639 mg), 2-chloro-3,4-difluorobenzonitrile (491 mg), lithium carbonate (669 mg) and dimethyl sulfoxide (13 mL) was stirred at 90° C. for 1 hr. The reaction mixture was cooled and partitioned between water and ethyl acetate. The organic layer was washed with water, dried over anhydrous sodium sulfate and concentrated. The obtained residue was purified by silica gel column chromatography (developing solvent: ethyl acetate-hexane). The obtained solid was recrystallized from ethyl acetate to give the title compound as crystals (yield: 538 mg).

1. temperatureThe reaction mixture was cooled
2. custompartitioned between water and ethyl acetate
3. washThe organic layer was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customThe obtained residue was purified by silica gel column chromatography (developing solvent: ethyl acetate-hexane)
7. customThe obtained solid was recrystallized from ethyl acetate