反应详情

4-Cyanomethyl-piperidine-4-carboxylic acid ethyl ester (14.2 g) was dissolved in pyridine (150 ml), 2-chlorobenzenesulfonyl chloride (16.83 g) was added and the reaction mixture was stirred overnight at RT. Then, most of pyridine was evaporated off in vacuo, the residue was dissolved in AcOEt, washed with 0.5M aqueous HCl and brine. The organic layer was dried over magnesium sulphate and concentrated in vacuo. The residue (crude oil) was chromatographed over silica (AcOEt/Heptanes, gradient from 0 to 25%) to give the desired material (8.5 g) as viscous brown oil. MS (ESI): 388.1 (M+NH4)+.

1. customThen, most of pyridine was evaporated off in vacuo
2. dissolutionthe residue was dissolved in AcOEt
3. washwashed with 0.5M aqueous HCl and brine
4. dry with materialThe organic layer was dried over magnesium sulphate
5. concentrationconcentrated in vacuo
6. customThe residue (crude oil) was chromatographed over silica (AcOEt/Heptanes, gradient from 0 to 25%)