반응 #83825

반응 방정식

potassium carbonate

2-(2-chloroethyl)-toluene-4-sulfonate

3-hydroxy-pyrid-2-ylsulfonamide

→

sulfonamide

수율 61.0%

3-(2-chloroethoxy)-pyrid-2-ylsulfonamide

수율 61.0%

용매

dimethylacetamide

반응 조건

후처리

1. 1
   온도cooled
2. 2
   여과filtered
3. 3
   세척The filtration residue is washed with acetonitrile
4. 4
   여과filtered
5. 5
   농축concentrated
6. 6
   기타a rotary evaporator
7. 7
   기타For purification the residue
8. 8
   기타is chromatographed on a silica gel column
9. 9
   기타Removal of the eluant
10. 10
    기타by evaporation

실험 절차

First 17.9 g of potassium carbonate and then 28.14 g of 2-(2-chloroethyl)-toluene-4-sulfonate are added, with stirring, to a solution of 17.4 g of 3-hydroxy-pyrid-2-ylsulfonamide in 240 ml of dimethylacetamide. The reaction mixture is stirred for 1.5 hours at 80° C. and then cooled and filtered. The filtration residue is washed with acetonitrile. The filtrate and the washing liquid are adjusted to pH 5-6 with trifluoroacetic acid, filtered and concentrated using a rotary evaporator. For purification the residue is chromatographed on a silica gel column using ethyl acetate/n-hexane 4/1. Removal of the eluant by evaporation yields 14.42 g of the above sulfonamide in the form of colourless crystals which melt at 136°-138° C.

출처