反应详情

To a solution of 334c (3.0 g, 14.6 mmol) in anhydrous DMF (30 mL) was added NaH (880 mg, 22 mmol). The mixture was stirred at room temperature for 30 minutes. 2-Bromoacetonitrile (3.5 g, 29.3 mmol) was added and the resulting mixture was heated at 65° C. for 1 hour. It was then cooled to room temperature and stirred for overnight. After reaction water (30 mL) was added and the reaction mixture was extracted with ethyl acetate (3×200 mL). The organic phase was evaporated to dryness. The residue was purified by column chromatography eluting with 20:1 methylene chloride/methanol to give 334d as a brown solid (2.6 g, 72%). MS: [M+H]+ 245.

1. temperaturethe resulting mixture was heated at 65° C. for 1 hour
2. temperatureIt was then cooled to room temperature
3. stirringstirred for overnight
4. additionwas added
5. extractionthe reaction mixture was extracted with ethyl acetate (3×200 mL)
6. customThe organic phase was evaporated to dryness
7. customThe residue was purified by column chromatography
8. washeluting with 20:1 methylene chloride/methanol