Hydrogen Peroxide → 2-Chloro-4,5-difluorobenzoic acid

HRID 374608

反応式

HRID 374608 の反応式
[OH:1]O.[Cl:3][C:4]1[CH:17]=[C:16]([F:18])[C:15]([F:19])=[CH:14][C:5]=1[C:6](C1C=CC=CC=1)=[O:7]>S(=O)(=O)(O)O>[Cl:3][C:4]1[CH:17]=[C:16]([F:18])[C:15]([F:19])=[CH:14][C:5]=1[C:6]([OH:7])=[O:1]

参加物

4

反応物 2

HCID 784Hydrogen PeroxideHCID 704945(2-Chloro-4,5-difluorophenyl)(phenyl)methanone

生成物 1

HCID 7371712-Chloro-4,5-difluorobenzoic acid収率 88%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

32 g of 20% hydrogen peroxide solution are added dropwise over 30 min to a solution of 37.8 g (0.15 mol) of 2-chloro-4,5-difluorobenzophenone in 400 g of 100% sulfuric acid in such a way that the temperature remains below 35° C. The reaction is complete after 7 h. The reaction mixture is then poured on to 1200 g of ice. Extraction of the mother liquor with methyl tert-butyl ether, isolation of the crude product from the extract and crystallization from water gives 17.0 g (0.0883 mol, 88%) of colorless 2-chloro-4,5-difluorobenzoic acid melting at 104.4°-105.8° C.

後処理

  1. customremains below 35° C
  2. extractionExtraction of the mother liquor with methyl tert-butyl ether, isolation of the crude product from the
  3. extractionextract
  4. customcrystallization from water

出典と根拠

ORDレコード
ord-8cd1f6bc4278422bb9c35eef57c43084
出典データセット
uspto-grants-1996_01
特許番号
US05481032

関連ノート

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