Acetic Acid → 3-Nitrobenzoic acid

HRID 746303

반응식

HRID 746303 반응식
[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]

참가 물질

5

반응물 2

HCID 176Acetic Acid2회HCID 74223-Nitrotoluene

생성물 1

HCID 84973-Nitrobenzoic acid수율 75.5%

시약·촉매·용매 2

HCID 61372Cobalt(II) acetate tetrahydrate촉매HCID 253881Sodium Bromide촉매

반응 조건

온도
5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-113f9be77a614b28a4bc4185a9bab510
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04603220

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