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Methanol → Methyl 3-(morpholinosulfonyl)benzoate

HRID 877599
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HRID 877599 반응식
[O:1]1[CH2:6][CH2:5][N:4]([S:7]([C:10]2[CH:11]=[C:12]([CH:16]=[CH:17][CH:18]=2)[C:13]([OH:15])=[O:14])(=[O:9])=[O:8])[CH2:3][CH2:2]1.OS(O)(=O)=O.[CH3:24]O>>[O:1]1[CH2:6][CH2:5][N:4]([S:7]([C:10]2[CH:11]=[C:12]([CH:16]=[CH:17][CH:18]=2)[C:13]([O:15][CH3:24])=[O:14])(=[O:9])=[O:8])[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 2574763-(Morpholine-4-sulfonyl)benzoic acid

생성물 1

HCID 779656Methyl 3-(morpholinosulfonyl)benzoate

실험 절차

3-(Morpholinosulfonyl)benzoic acid (100 mg, 0.369 mmol) was refluxed overnight in methanol in the presence of catalytic concentrated H2SO4 at 65° C. The reaction was monitored by TLC. After completion of the reaction, the solvent was removed by vacuum and then compound was purified by column chromatography to yield the title compound as an off white solid (60 mg). 1H NMR (400 MHz, CDCl3): δ 8.38 (t, 1H, J=1.6 Hz), 8.27 (m, 1H), 7.92 (m, 1H), 7.64 (t, 1H, J=8.0 Hz), 3.95 (s, 3H), 3.73 (m, 4H), 3.00 (m, 4H). ESI-MS: 286.1 [M+H]+.

후처리

  1. customAfter completion of the reaction
  • customthe solvent was removed by vacuum
  • customcompound was purified by column chromatography
  • 출처 및 근거

    ORD 기록
    ord-44c5d39c81284701a3faf3cdebbfc980
    출처 데이터셋
    uspto-grants-2015_03
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08987335B2

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