反应详情

温度

0 °C

A solution of trans-4-{[2,5-bis-(2,2,2-trifluoro-ethoxy)-benzenesulfonylamino]-methyl}-cyclohexanecarboxylic acid (2.78 g, 5.63 mmol) and triethylamine (1.9 mL, 13.6 mmol) in THF (25 mL) was cooled to 0° C. To the mixture was added ethyl chloroformate (0.586 mL, 6.2 mmol) in THF (5 mL) over 10 min. After stirring at 0° C. for 15 min, 25% aqueous ammonia (10 mL) was added dropwise. The mixture was stirred at ambient temperature for 2 hr. The resulting mixture was concentrated under reduced pressure and the concentrate was diluted with water to give a solid. The solid was filtered and washed with water and hexanes to give trans-4-{[2,5-bis-(2,2,2-trifluoro-ethoxy)-benzenesulfonylamino]-methyl}-cyclohexanecarboxylic acid amide as a white solid (2.7 g, 98%).

1. stirringThe mixture was stirred at ambient temperature for 2 hr
2. concentrationThe resulting mixture was concentrated under reduced pressure
3. additionthe concentrate was diluted with water
4. customto give a solid
5. filtrationThe solid was filtered
6. washwashed with water and hexanes