反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A 842 mg portion of 4-(acetylamino)benzene sulfonyl chloride was added under ice-cooling to a pyridine solution (10 ml) of 3-(piperidin-2-yl)pyridine and stirred at room temperature for 2 hours. The solvent was concentrated under a reduced pressure, and the thus obtained residue was mixed with ethyl acetate and then washed with water, 1 M hydrochloric acid and saturated brine. This was dried with anhydrous sodium sulfate and then concentrated under a reduced pressure, and the thus obtained residue was purified by a silica gel column chromatography using chloroform:methanol (98:2) as the elution solvent, thereby obtaining 1.00 g of N-(4-{[2-(pyridin-3-yl)piperidin-1-yl]sulfonyl}phenyl)acetamide as a yellow foamy substance. FAB-MS (Pos): 360 [M+H]+.
WORKUP
后处理
- concentrationThe solvent was concentrated under a reduced pressure
- additionthe thus obtained residue was mixed with ethyl acetate
- washwashed with water, 1 M hydrochloric acid and saturated brine
- dry with materialThis was dried with anhydrous sodium sulfate
- concentrationconcentrated under a reduced pressure
- customthe thus obtained residue was purified by a silica gel column chromatography