反应详情

3-Methoxybenzenesulfonyl chloride (331 mg, 1.6 mmol) was added to a solution of 1-(4′-chloro-2′-fluoro-1,1′-biphenyl-2-yl)ethylamine (400 mg, 1.6 mmol) and triethylamine (246 μL, 1.7 mmol) in acetonitrile. The reaction was mixed at room temperature for 24 hours, afterwhich the acetonitrile was removed in vacuo. The remaining solid was dissolved in dichloromethane and purified by preparative liquid chromatogrpahy on a Biotage® 40 Mi column of prepacked silica gel (90 g), eluting with a gradient of 5%-50% methyl tert-butyl ether in hexane (35 min), to afford the the desired product (694 mg, 99%) as a white solid;

1. customwas removed in vacuo
2. dissolutionThe remaining solid was dissolved in dichloromethane
3. custompurified by preparative liquid chromatogrpahy on a Biotage® 40 Mi column of prepacked silica gel (90 g)
4. washeluting with a gradient of 5%-50% methyl tert-butyl ether in hexane (35 min)