반응 #2502

반응 방정식

sodium carbonate

pyridine

o-Anisidine

3-pyridinesulfonylchloride hydrochloride

→

title compound

수율 83.5%

N-(2-Methoxyphenyl)-3-pyridinesulfonamide

수율 83.5%

용매

water

toluene

반응 조건

후처리

1. 1
   기타at room temperature
2. 2
   기타the resulting reaction solution
3. 3
   추출extracted with ethyl acetate
4. 4
   세척washed with water and saturated brine
5. 5
   건조After drying on anhydrous sodium carbonate
6. 6
   기타removing the solvent
7. 7
   기타by evaporation
8. 8
   기타the resulting orange solid was purified by a silica gel column chromatography (ether:hexane=3:1)
9. 9
   기타to obtain a light orange solid which
10. 10
    세척was subsequently washed with an ether-hexane (1:3) mixture solution

실험 절차

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.

출처