反应详情

A solution of 3,4,5-trifluoronitrobenzene (5.00 g, 28.24 mmol) in acetonitrile (60 mL) is cooled to 0° C. and treated with N,N-diisopropylethylamine (7.38 mL, 42.35 mmol) followed by thiomorpholine (2.98 mL, 29.65 mmol). The ice bath is removed and the reaction mixture stirred at room temperature under nitrogen for approximately 24 h, during which additional thiomorpholine (0.1 eq) is added. The solvent is removed under reduced pressure, and the residue is diluted with ethyl acetate, washed with 1N hydrochloric acid (until the washings are acidic), saturated aqueous sodium bicarbonate and saline, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give the title compound, mp 104–105° C.

1. customThe ice bath is removed
2. additionis added
3. customThe solvent is removed under reduced pressure
4. additionthe residue is diluted with ethyl acetate
5. washwashed with 1N hydrochloric acid (until the washings
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated under reduced pressure