Methanol → 4-(Methanesulfonyl)-3-nitrobenzoic acid

HRID 1785330ノート

反応式

HRID 1785330 の反応式
CS[C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][C:4]=1[N+:12]([O-:14])=[O:13].O[O:16][S:17]([O-:19])=O.[K+].[CH3:21]O>O>[CH3:21][S:17]([C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][C:4]=1[N+:12]([O-:14])=[O:13])(=[O:19])=[O:16]

参加物

5

反応物 3

HCID 887MethanolHCID 5425314-Methylthio-3-nitrobenzoic acidHCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 27238714-(Methanesulfonyl)-3-nitrobenzoic acid収率 89%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
5 °C

実験手順

4-Methylsulfanyl-3-nitro-benzoic acid (1 g, 4.69 mmole) was dissolved in methanol (25 ml) and cooled to 5° C. A solution of Oxone® (5.8 g) in water (20 ml) was added portionwise at the same temperature. The reaction mixture was allowed to stir overnight at ambient temperature, methanol was removed under reduced pressure. The suspension was diluted with water and the solid was filtered off and dried in vacuum to provide 4-Methanesulfonyl-3-nitro-benzoic acid in 89% yield (960 mg). ESI-MS: 246.

後処理

  1. custommethanol was removed under reduced pressure
  2. additionThe suspension was diluted with water
  3. filtrationthe solid was filtered off
  4. customdried in vacuum

出典と根拠

ORDレコード
ord-78753cfe6dbd453bb7a910a347da8ed0
出典データセット
uspto-grants-2009_03
特許番号
US07504410B2

反応ノート

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