反应 #2502

反应方程式

sodium carbonate

pyridine

o-Anisidine

3-pyridinesulfonylchloride hydrochloride

→

title compound

收率 83.5%

N-(2-Methoxyphenyl)-3-pyridinesulfonamide

收率 83.5%

溶剂

water

toluene

反应条件

后处理

1. 1
   其他at room temperature
2. 2
   其他the resulting reaction solution
3. 3
   萃取extracted with ethyl acetate
4. 4
   洗涤washed with water and saturated brine
5. 5
   干燥After drying on anhydrous sodium carbonate
6. 6
   其他removing the solvent
7. 7
   其他by evaporation
8. 8
   其他the resulting orange solid was purified by a silica gel column chromatography (ether:hexane=3:1)
9. 9
   其他to obtain a light orange solid which
10. 10
    洗涤was subsequently washed with an ether-hexane (1:3) mixture solution

实验过程

o-Anisidine (377 mg, 3.0 mmol) was dissolved in toluene (10 ml) to which were subsequently added pyridine (0.48 ml, 6.0 mmol) and 3-pyridinesulfonylchloride hydrochloride (642 mg, 3.0 mmol) at room temperature. After 1.5 hours of stirring at 100° C., the resulting reaction solution was mixed with water (20 ml), adjusted to pH 7 to 8 with anhydrous sodium carbonate, extracted with ethyl acetate and then washed with water and saturated brine. After drying on anhydrous sodium carbonate and removing the solvent by evaporation, the resulting orange solid was purified by a silica gel column chromatography (ether:hexane=3:1) to obtain a light orange solid which was subsequently washed with an ether-hexane (1:3) mixture solution to obtain 662 mg (83.5%) of the title compound in the form of colorless prism crystals.

来源