Methanol → Methyl 3-(dimethylsulfamoyl)benzoate

HRID 877608ノート

反応式

HRID 877608 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

HCID 1262217Methyl 3-(dimethylsulfamoyl)benzoate

実験手順

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]+.

後処理

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

出典と根拠

ORDレコード
ord-df478f5fe3d74dc29b77ac33dd68c4c2
出典データセット
uspto-grants-2015_03
特許番号
US08987335B2

反応ノート

読み込み中…