Sulfuric Acid → 2-Chloro-4,5-difluorobenzoic acid

HRID 374613

反応式

HRID 374613 の反応式
[NH4+].[NH4+].[O-]S(OOS([O-])(=O)=O)(=O)=O.[Cl:13][C:14]1[CH:27]=[C:26]([F:28])[C:25]([F:29])=[CH:24][C:15]=1[C:16](C1C=CC=CC=1)=[O:17].S(=O)(=O)(O)[OH:31]>C(O)(=O)C>[Cl:13][C:14]1[CH:27]=[C:26]([F:28])[C:25]([F:29])=[CH:24][C:15]=1[C:16]([OH:17])=[O:31]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 62648Ammonium PersulfateHCID 704945(2-Chloro-4,5-difluorophenyl)(phenyl)methanone

生成物 1

HCID 7371712-Chloro-4,5-difluorobenzoic acid収率 80.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

8 g of ammonium peroxodisulfate are introduced into 5 g (19.8 mmol ) of 2-chloro-4,5-difluorobenzophenone and 20 g of glacial acetic acid and the mixture is heated at 90° C. (12 h). 100 g of 70% sulfuric acid are then added and the mixture is heated for 2 h at 150° C. Dilution with 200 g of water and filtration gives 3.1 g (16.0 mmol, 81%) of 2-chloro-4,5-difluorobenzoic acid (purity (GC) ca. 92%). Recrystallization from water gives 2.5 g of product melting at 104° C.-105° C.

後処理

  1. temperaturethe mixture is heated for 2 h at 150° C
  2. filtrationDilution with 200 g of water and filtration

出典と根拠

ORDレコード
ord-57ce944fb97645a09a59dd154d8b1826
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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