反应详情

温度

0 °C

Dimethylaminopyridine (1.83 g, 15 mmol, 0.05 eq) and triethylamine (63.5 ml, 450 mmol, 1.5 eq) are added to a solution of 1-[2-(2-hydroxyethyl)phenyl]piperidin-2-one a2-2 (65.7 g, 300 mmol, 1 eq) in dichloromethane (250 ml) at 0° C. The mixture is stirred at 0° C. for 15 minutes, then a solution of 4-toluenesulfonyl chloride (63 g, 330 mmol, 1.1 eq) in dichloromethane (250 ml) is added dropwise. The reaction mixture is then warmed up to room temperature and stirred overnight. The reaction mixture is washed with water, 1N HCl, then dried over MgSO4, filtered and evaporated under vacuum. The residue is purified by chromatography over silicagel (gradient: CH2Cl2/MeOH from 100/0 to 98/2) to afford 99 g of 2-[2-(2-oxopiperidin-1-yl)phenyl]ethyl 4-methylbenzenesulfonate a2-3.

1. temperatureThe reaction mixture is then warmed up to room temperature
2. stirringstirred overnight
3. washThe reaction mixture is washed with water, 1N HCl
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customevaporated under vacuum
7. customThe residue is purified by chromatography over silicagel (gradient: CH2Cl2/MeOH from 100/0 to 98/2)