Potassium Carbonate → 2-Fluoro-6-nitrobenzoic acid

HRID 67448

反応式

HRID 67448 の反応式
[F:1][C:2]1[C:7](C)=[C:6]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:4][CH:3]=1.[C:12](=[O:15])([O-])[O-:13].[K+].[K+].[Mn]([O-])(=O)(=O)=O.[K+].[Mn]([O-])(=O)(=O)=O>O>[F:1][C:2]1[C:7]([C:12]([OH:13])=[O:15])=[C:6]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 24401PermanganateHCID 698542-Fluoro-6-nitrotolueneHCID 516875Potassium Permanganate

生成物 1

HCID 6037582-Fluoro-6-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 34.5 g (0.22 mol) of 6-fluoro-2-nitrotoluene, 30.7 g (0.22 mol) of potassium carbonate, 105.4 g (0.66 mol) of potassium permanganate and 3.3 liters of water is heated at 100° C. until the permanganate is decolorised (ca 2.5 hours). After cooling and removal of the unreacted 6-fluoro-2-nitrotoluene by extraction with ethyl acetate, the aqueous phase is adjusted to pH 1 with hydrochloric acid and extracted three times with ethyl acetate. The combined organic extracts are dried over magnesium sulphate and concentrated, there being obtained 6-fluoro-2-nitrobenzoic acid. After recrystallisation from ethyl acetate/n-hexane, the product melts at 146°-148° C.

後処理

  1. custom(ca 2.5 hours)
  2. temperatureAfter cooling
  3. customremoval of the unreacted 6-fluoro-2-nitrotoluene
  4. extractionby extraction with ethyl acetate
  5. extractionextracted three times with ethyl acetate
  6. dry with materialThe combined organic extracts are dried over magnesium sulphate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-71286dd7ff0f4e78829969ad2bf5f4c2
出典データセット
uspto-grants-1982_08
特許番号
US04346034

関連ノート

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