反应详情

A solution of piperazine (24 g, 0.28 mol) and 3,4,5-trifluoronitrobenzene (13 mL, 0.11 mol) in acetonitrile (200 mL) was stirred at 60° C. The progress of reaction was monitored by TLC. On completion, acetonitrile was evaporated under reduced pressure. The residue was dissolved in ethyl acetate (300 mL) and resulting solution was washed with water (100 mL), brine (100 mL), dried over anhydrous sodium sulphate and concentrated in vacuo. The residue was purified by column chromatography (silica gel, 1:9 methanol:chloroform) to provide title compound (25.8 g, 92%) as orange solid.

1. customThe progress of reaction
2. customOn completion, acetonitrile was evaporated under reduced pressure
3. dissolutionThe residue was dissolved in ethyl acetate (300 mL)
4. customresulting solution
5. washwas washed with water (100 mL), brine (100 mL)
6. dry with materialdried over anhydrous sodium sulphate
7. concentrationconcentrated in vacuo
8. customThe residue was purified by column chromatography (silica gel, 1:9 methanol:chloroform)