Methanol → Methyl 3-(dimethylsulfamoyl)benzoate

HRID 877608노트

반응식

HRID 877608 반응식
[CH3:1][N:2]([CH3:15])[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.[CH3:21]O>>[CH3:1][N:2]([CH3:15])[S:3]([C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][CH:14]=1)[C:9]([O:11][CH3:21])=[O:10])(=[O:4])=[O:5]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 49857623-(N,N-dimethylsulfamoyl)benzoic acid

생성물 1

HCID 1262217Methyl 3-(dimethylsulfamoyl)benzoate

실험 절차

3-(N,N-Dimethylsulfamoyl)benzoic acid (200 mg, 0.872 mmol) was refluxed overnight in the presence of concentrated sulfuric acid (5.64 mg, 0.044 mmol) in methanol (10 mL) at 70° C. Reaction was monitored by TLC. After completion of the reaction, the solvent was removed by vacuum and then compound was purified by column chromatography affording the title compound (125 mg). 1H NMR (400 MHz, CDCl3): δ 8.42 (s, 1H), 8.27 (d, 1H, J=8.0 Hz), 7.97 (d, 1H, J=7.2 Hz), 7.65 (t, 1H, J=8.0 Hz), 3.96 (s, 3H), 2.74 (s, 6H). ESI-MS: 244.0 [M+H]+.

후처리

  1. customReaction
  2. customAfter completion of the reaction
  3. customthe solvent was removed by vacuum
  4. customcompound was purified by column chromatography

출처 및 근거

ORD 기록
ord-df478f5fe3d74dc29b77ac33dd68c4c2
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987335B2

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