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Methanol → Methyl 2-[(3-hydroxypropyl)sulfonyl]-5-sulfamoylbenzoate

HRID 2118580
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HRID 2118580 반응식
[OH:1][CH2:2][CH2:3][CH2:4][S:5][C:6]1[CH:11]=[CH:10][C:9]([S:12]([NH2:15])(=[O:14])=[O:13])=[CH:8][C:7]=1[C:16]([OH:18])=[O:17].OS(O)(=O)=O.[CH3:24]O>>[OH:1][CH2:2][CH2:3][CH2:4][S:5][C:6]1[CH:11]=[CH:10][C:9]([S:12]([NH2:15])(=[O:14])=[O:13])=[CH:8][C:7]=1[C:16]([O:18][CH3:24])=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 13960351HCID 13960351, 화합물

생성물 1

HCID 13960352Methyl 2-[(3-hydroxypropyl)sulfonyl]-5-sulfamoylbenzoate

실험 절차

4-(3-hydroxypropylthio)-3-carboxybenzene-sulfonamide (15 g, 0.0515 mol) and concentrated H2SO4 (4 ml) were dissolved in methanol (150 ml) and refluxed on a steam bath for about 5 hours. The solvent was removed and the residue was treated with water. The mixture was extracted with ethylacetate, which was washed with water, saturated sodium bicarbonate, water and brine. After drying, removal of the solvent left a tannish solid. Recrystallization from 1,2-dichloroethane gave 13.5 g of a white solid. M.p.=123°-125°.

후처리

  1. temperaturerefluxed on a steam bath for about 5 hours
  • customThe solvent was removed
  • additionthe residue was treated with water
  • extractionThe mixture was extracted with ethylacetate, which
  • washwas washed with water, saturated sodium bicarbonate, water and brine
  • customAfter drying
  • customremoval of the solvent
  • waitleft a tannish solid
  • customRecrystallization from 1,2-dichloroethane
  • 출처 및 근거

    ORD 기록
    ord-6f0fe8d684c841c9b62bd4e57bf96653
    출처 데이터셋
    uspto-grants-1987_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04678855

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