反应 #57807

反应方程式

4-Bromo-benzenesulfonyl chloride

(2-amino-5-chloro-phenyl)-pyridin-4-yl-methanone

→

4-Bromo-N-[4-chloro-2-(pyridine-4-carbonyl)-phenyl]-benzenesulfonamide

溶剂

pyridine

反应条件

后处理

1. 1
   其他pyridine was then evaporated under vacuum
2. 2
   workup.DISSOLUTIONThe resulting crude material was dissolved in dichloromethane
3. 3
   萃取extracted with saturated bicarbonate solution
4. 4
   洗涤The combined organic layer was washed with brine
5. 5
   干燥dried over magnesium sulfate
6. 6
   过滤filtered
7. 7
   浓缩concentrated
8. 8
   workup.ADDITIONethyl acetate (50 mL) added to the solid
9. 9
   过滤the solid was filtered
10. 10
    洗涤washed again with ethyl acetate
11. 11
    其他to yield a pale yellow solid

实验过程

4-Bromo-benzenesulfonyl chloride 27.5 g (107 mmol) was dissolved in 180 ml of anhydrous pyridine. To this solution was added (2-amino-5-chloro-phenyl)-pyridin-4-yl-methanone 25 g (107 mmol). The reaction mixture was stirred under nitrogen 5 hour at 80° C. and pyridine was then evaporated under vacuum. The resulting crude material was dissolved in dichloromethane, and extracted with saturated bicarbonate solution. The combined organic layer was washed with brine dried over magnesium sulfate, filtered and concentrated, then ethyl acetate (50 mL) added to the solid, the solid was filtered, washed again with ethyl acetate, to yield a pale yellow solid: LC-MSD, m/z for C18H12BrClN2O3S [M+H]+: 452.9

来源