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Sulfuric Acid → 3-Isobutylamino-2-methyl-4-(methylsulfonyl)benzoic acid

HRID 547247
ノート
印刷プレビュー

反応式

HRID 547247 の反応式
F[C:2]1[C:3]([CH3:15])=[C:4]([CH:8]=[CH:9][C:10]=1[S:11]([CH3:14])(=[O:13])=[O:12])[C:5]([OH:7])=[O:6].[CH2:16]([NH2:20])[CH:17]([CH3:19])[CH3:18].S(=O)(=O)(O)O>>[CH2:16]([NH:20][C:2]1[C:3]([CH3:15])=[C:4]([CH:8]=[CH:9][C:10]=1[S:11]([CH3:14])(=[O:13])=[O:12])[C:5]([OH:7])=[O:6])[CH:17]([CH3:19])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 6558IsobutylamineHCID 142544793-Fluoro-2-methyl-4-(methylsulfonyl)benzoic acid

生成物 1

HCID 574365663-Isobutylamino-2-methyl-4-(methylsulfonyl)benzoic acid

実験手順

2.0 g (9 mmol) of 3-fluoro-2-methyl-4-(methylsulfonyl)benzoic acid were dissolved in 26.5 ml (267 mmol) of isobutylamine. The mixture was heated at reflux with stirring for 8 days, cooled to RT, acidified with 10% strength sulfuric acid and extracted twice with ethyl acetate. The combined organic phases were dried over MgSO4, and the solvent was removed under reduced pressure. This gave 2.4 g of a colorless solid of a purity of 98%.

後処理

  1. temperature
The mixture was heated
  • temperatureat reflux
  • extractionextracted twice with ethyl acetate
  • dry with materialThe combined organic phases were dried over MgSO4
  • customthe solvent was removed under reduced pressure
  • 出典と根拠

    ORDレコード
    ord-d0da8512be5e44a8bb6f2c4e224bc5ff
    出典データセット
    uspto-grants-2011_05
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US07939467B2

    反応ノート

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