反应详情

温度

100 °C

Bicyclo[3.2.1]octan-2-one (2 g) and 4-fluorobenzoylacetonitrile (2.6 g) are dissolved in 1,1,2,2-tetrachloroethane (5 ml) and thereto is added 75% polyphosphoric acid (25 g). The mixture is stirred at 80° C. for 30 minutes, at 100° C. for 1 hour, and further at 130° C. for 30 minutes. After cooling, the reaction mixture is poured into ice-water and neutralized with potassium carbonate. The precipitated crystals are collected by filtration and washed successively with water and ethyl acetate. The resultant is recrystallized from methanol to give the desired product (2.7 g), m.p.>300° C.

1. waitfurther at 130° C. for 30 minutes
2. temperatureAfter cooling
3. filtrationThe precipitated crystals are collected by filtration
4. washwashed successively with water and ethyl acetate
5. customThe resultant is recrystallized from methanol