Acetic Acid → 3-Nitrobenzoic acid

HRID 746303

反応式

HRID 746303 の反応式
[N+:1]([C:4]1[CH:5]=C(C)[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[C:11]([OH:14])(=[O:13])[CH3:12]>O.O.O.O.C([O-])(=O)C.[Co+2].C([O-])(=O)C.[Br-].[Na+]>[N+:1]([C:4]1[CH:5]=[C:12]([CH:7]=[CH:8][CH:9]=1)[C:11]([OH:14])=[O:13])([O-:3])=[O:2]

参加物

5

反応物 2

HCID 176Acetic Acid2 回HCID 74223-Nitrotoluene

生成物 1

HCID 84973-Nitrobenzoic acid収率 75.5%

試薬・触媒・溶媒 2

HCID 61372Cobalt(II) acetate tetrahydrate触媒HCID 253881Sodium Bromide触媒

反応条件

温度
5 °C

実験手順

Similarly to Example 1, 250 g of m-nitrotoluene was oxidized in the presence of 150 g of acetic acid, 4.5 g of cobalt acetate tetrahydrate and 2 g of sodium bromide at a pressure of 25 bar, a temperature of 135°-145° C. and a gas exhaust rate of 3 1/min, within a period of 200 minutes. The reaction mixture, diluted with 400 g of 69% acetic acid, was cooled to 5° C. with stirring, filtered, twice washed with 125 g of 50% acetic acid at 5° C. and once with 150 g of water, the mother liquor (514.5 g) and the combined washing filtrates (441 g) being recovered separately. After drying, 230 g of m-nitrobenzoic acid was obtained.

後処理

  1. filtrationfiltered
  2. washtwice washed with 125 g of 50% acetic acid at 5° C. and once with 150 g of water
  3. washthe mother liquor (514.5 g) and the combined washing filtrates (441 g)
  4. custombeing recovered separately
  5. customAfter drying

出典と根拠

ORDレコード
ord-113f9be77a614b28a4bc4185a9bab510
出典データセット
uspto-grants-1986_07
特許番号
US04603220

関連ノート

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