反应详情

温度

105 °C

To a solution of 5-(3,3-difluoroazetidin-1-yl)-4-(2,2,2-trifluoroethoxy)pyridine-2-carbonitrile (example 223a, 680 mg, 2.32 mmol) in EtOH (8 ml) in a schlenk tube was added a 4M aqueous solution of potassium hydroxide (651 mg, 11.6 mmol). The reaction mixture was stirred at 105° C. for 2 hours. The reaction mixture was diluted with ethyl acetate and poured in a separatory funnel. The organic phase was extracted with a 1M aqueous solution of hydrochloric acid. The organic phase was collected and the aqueous phase was back-extracted with ethyl acetate. Combined organic phases were dried over sodium sulfate and evaporated down to dryness to yield the title compound (397 mg, 55%) as a crude solid which was used without any purification. MS (ESI, m/z): 311.2 (M−H+).

1. additionpoured in a separatory funnel
2. extractionThe organic phase was extracted with a 1M aqueous solution of hydrochloric acid
3. customThe organic phase was collected
4. extractionthe aqueous phase was back-extracted with ethyl acetate
5. dry with materialCombined organic phases were dried over sodium sulfate
6. customevaporated down to dryness