反应详情

温度

35 °C

To 4 g (12.4 mmol) trans-N-(4-Hydroxy-cyclohexyl)-4-trifluoromethyl-benzenesulfonamide in 20 ml DMF were added 5.1 g (37.1 mmol, 3.3 eq) K2CO3 and 2.04 ml (27.2 mmol, 2.2 eq) ethyl bromide. The mixture was stirred at 35° C. over night, concentrated in vacuo and dissolved in CH2Cl2 and water. The phases were separated and the inorganic one was extracted CH2Cl2, the combined organic phases were washed with brine and dried over Na2SO4. The crude product was purified by column chromatography on silica gel with CH2Cl2/MeOH 95:5 to yield 1.6 g (38%) trans-N-Ethyl-N-(4-hydroxy-cyclohexyl)-4-trifluoromethyl-benzenesulfonamide as brown oil, MS: 351(M).

1. concentrationconcentrated in vacuo
2. dissolutiondissolved in CH2Cl2
3. customThe phases were separated
4. extractionthe inorganic one was extracted CH2Cl2
5. washthe combined organic phases were washed with brine
6. dry with materialdried over Na2SO4
7. customThe crude product was purified by column chromatography on silica gel with CH2Cl2/MeOH 95:5