反应详情

温度

25 °C

To a solution of 3,3,3-trifluoro-2-(trifluoromethyl)-1-(hydroxymethyl)propyl amine (79 mg, 0.374 mmol) in CH2Cl2 (1 mL) was added triethylamine (0.1 mL, 0.749 mmol) and 4-fluorobenzenesulfonyl chloride (80.5 mg, 0.4 mmol) in CH2Cl2 (1 mL). The solution was stirred for 20 hours at 25° C. and then concentrated. EtOAc (5 mL) was added and the solution was washed with 1M HCl (1 mL), brine (1 mL), dried over Na2SO4 and concentrated. The crude solid was purified by Biotage Flash™ chromatography, eluting with EtOAc/hexanes (1:4), to give 4-fluoro-N-[3,3,3-trifluoro-1-(hydroxymethyl)-2-(trifluoromethyl)propyl]benzene sulfonamide (2.5 mg) as a white solid.

1. concentrationconcentrated
2. additionEtOAc (5 mL) was added
3. washthe solution was washed with 1M HCl (1 mL), brine (1 mL)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe crude solid was purified by Biotage Flash™ chromatography
7. washeluting with EtOAc/hexanes (1:4)