反应详情

A solution of 2.08 ml (13.07 mmol) diisopropylamine in dry THF (12 ml) was cooled to −70° C. under inert gas atmosphere, and 9.26 ml (14.8 mmol) n-butyllithium solution (1.6 M in hexanes) were added dropwise. Then, a solution of 688 μl (13.07 mmol) acetonitrile in dry THF (10 ml) was slowly added over 10 min. The resulting solution was stirred for further 30 min at −70° C. before a solution of 1.50 g (8.72 mmol) 6-(trifluoromethyl)pyridine-2-carbonitrile in dry THF (10 ml) was added. The mixture was allowed to warm to room temperature and stirred for 12 h before water (200 ml) was added slowly. The mixture was extracted several times with dichloromethane (100 ml). The combined organic layers were dried over sodium sulfate and concentrated under reduced pressure to yield 1.2 g (57% of th.) of the crude title compound (89% purity) which was used in the next step without further purification.

1. additionwere added dropwise
2. additionwas added
3. additionwas added slowly
4. extractionThe mixture was extracted several times with dichloromethane (100 ml)
5. dry with materialThe combined organic layers were dried over sodium sulfate
6. concentrationconcentrated under reduced pressure