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Methanol → methyl 3-(N-methylsulfamoyl)benzoate

HRID 1777048
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HRID 1777048 반응식
[CH3:1][NH:2][S:3]([C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][CH:14]=1)[C:9]([OH:11])=[O:10])(=[O:5])=[O:4].S(=O)(=O)(O)O.[CH3:20]O>>[CH3:1][NH:2][S:3]([C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][CH:14]=1)[C:9]([O:11][CH3:20])=[O:10])(=[O:4])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 2526543-(Methylsulfamoyl)benzoic acid

생성물 1

HCID 9320906methyl 3-(N-methylsulfamoyl)benzoate수율 53.5%

실험 절차

3-(N-methylsulfamoyl)benzoic acid (200 mg, 0.929 mmol) was refluxed in the presence of concentrated sulfuric acid (6.01 mg, 0.046 mmol) in methanol at 70° C. for overnight. Reaction was monitored by TLC. After completion of the reaction, the solvent was removed by vacuum and then compound was purified by flash chromatography afforded the methyl 3-(N-methylsulfamoyl)benzoate (120 mg, 0.497 mmol, 53.5% yield). 1H NMR (CDCl3, 400 MHz): δ 8.51 (m, 1H), 8.25 (m, 1H), 8.06 (dt, 1H, J=1.2 & 8.0 Hz), 7.63 (t, 1H, J=7.6 Hz), 3.96 (s, 3H), 2.69 (s, 3H). Mass [M+H]+: 230.1

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이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
  • customReaction
  • customAfter completion of the reaction
  • customthe solvent was removed by vacuum
  • customcompound was purified by flash chromatography
  • 출처 및 근거

    ORD 기록
    ord-fd325ed1e31d4c07961251daafc6691a
    출처 데이터셋
    uspto-grants-2016_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US09266838B2

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