反应详情

Under reflux, 1.7 g of sodium (72.8 mmol) was dissolved in 50 ml of ethanol. At 50° C., a solution of 14.2 g (72.8 mmol) of 2-(7-chloro-1,3-benzodioxol-5-yl)acetonitrile and 10.3 g (72.8 mmol) of ethyl trifluoroacetate in 50 ml of ethanol was added dropwise, and the reaction mixture was then stirred under reflux for 12 hours. After cooling, the reaction mixture was concentrated on a rotary evaporator, dissolved in ethyl acetate and washed twice with 100 ml of 1N hydrochloric acid and once with water. The organic phase was separated off, dried over sodium sulphate, filtered and concentrated to give the title compound (23.9 g; 100%) and used for the next step directly.

1. temperatureUnder reflux
2. temperatureunder reflux for 12 hours
3. temperatureAfter cooling
4. concentrationthe reaction mixture was concentrated on a rotary evaporator
5. dissolutiondissolved in ethyl acetate
6. washwashed twice with 100 ml of 1N hydrochloric acid and once with water
7. customThe organic phase was separated off
8. dry with materialdried over sodium sulphate
9. filtrationfiltered
10. concentrationconcentrated