Methanol → Methyl 3-(morpholinosulfonyl)benzoate

HRID 877599

반응식

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 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
  2. customthe solvent was removed by vacuum
  3. customcompound was purified by column chromatography

출처 및 근거

ORD 기록
ord-44c5d39c81284701a3faf3cdebbfc980
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987335B2

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