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With ammonium hydroxide In tetrahydrofuran at 20℃;
To a solution of 2,4,5-trifluorobenzene-1-sulfonyl chloride (3.0 g, 13 mmol), in THF(30 mL) was added NH4OH (910 mg, 26 mmol) and the solution was stirred for 14 h at rt. The solution was concentrated in vacuo to afford 2,4,5-trifluorobenzenesulfonamide (2.7 g, 13 mmol, 98percent) as a yellow solid. ESI-MS (EI+, m/z): 211.9 [M+H]t
With ammonium hydroxide In tetrahydrofuran at 20℃;
13.1 Step 1: 2,4,5-trifluorobenzenesulfonamide
To a solution of 2,4,5-trifluorobenzene-1-sulfonyl chloride (3.0 g, 13 mmol), in THF(30 mL) was added NH4OH (910 mg, 26 mmol) and the solution was stirred for 14 h at rt. The solution was concentrated in vacuo to afford 2,4,5-trifluorobenzenesulfonamide (2.7 g, 13 mmol, 98%) as a yellow solid. ESI-MS (EI+, m/z): 211.9 [M+H]t
2,4,5-trifluoro-N-(methylcarbamoyl)benzenesulfonamide[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
70.5%
With 1,8-diazabicyclo[5.4.0]undec-7-ene; In acetonitrile; for 8h;Reflux;
Add 2,4,5-trifluoro-benzenesulfonamide (10.0g, 47.357mmol) and dry acetonitrile (50mL) to the reaction flask, stir and mix well, add phenyl carbamate (7.9g, 52.291mmol), then DBU (10.86g, 71.306mmol) was added dropwise. After the addition was completed, the reaction was heated to reflux for 8 hours. The solvent was distilled off under reduced pressure. The residue was dissolved in ethyl acetate (300mL). Washed with an aqueous solution of sodium chloride (60 mL x 2), dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The resulting crude product was recrystallized from a mixed solvent of n-hexane / ethyl acetate to obtain 2,4,5-trifluoro-N- ( Carbamoyl) -benzenesulfonamide, yield 70.5%,
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