Acetic Acid → 4-Nitrobenzaldehyde

HRID 9753

반응식

HRID 9753 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].[OH:11]N1C(=O)N(O)C(=O)N(O)C1=O.[C:23]([OH:26])(=[O:25])[CH3:24]>C([O-])(=O)C.[Co+2].C([O-])(=O)C.C([O-])(=O)C.[Mn+2].C([O-])(=O)C.O>[N+:1]([C:4]1[CH:9]=[CH:8][C:24]([C:23]([OH:26])=[O:25])=[CH:6][CH:5]=1)([O-:3])=[O:2].[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH:10]=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2]

참가 물질

8

반응물 3

HCID 176Acetic AcidHCID 74734-NitrotolueneHCID 104197231,3,5-Trihydroxy-1,3,5-triazinane-2,4,6-trione

생성물 2

HCID 5414-NitrobenzaldehydeHCID 61084-Nitrobenzoic Acid

시약·촉매·용매 3

HCID 6277Cobalt diacetate촉매HCID 12525Manganous Acetate촉매HCID 962Water용매

반응 조건

온도
130 °C

실험 절차

In an autoclave, 0.274 g of 4-nitrotoluene, 0.011 g of hexahydro-1,3,5-trihydroxy-1,3,5-triazine-2,4,6-trione (3% by mole relative to 4-nitrotoluene), 5 g of acetic acid, 0.003 g of cobalt(II) acetate.4H2O and 0.001 g of manganese(II) acetate.4H2O were placed. The autoclave was charged with 1 MPa of air and placed in a heated oil bath. The mixture was stirred at 130° C. for 14 hours. After the completion of reaction, the autoclave was placed on cold water to cool down the reaction mixture quickly. The resulting mixture was analyzed by gas chromatography and was found to yield 4-nitrobenzoic acid and 4-nitrobenzaldehyde in 85% and 1% yields, respectively, at 91% conversion of 4-nitrotoluene.

후처리

  1. additionThe autoclave was charged with 1 MPa of air
  2. customplaced in a heated oil bath
  3. customAfter the completion of reaction
  4. temperatureto cool down the reaction mixture quickly

출처 및 근거

ORD 기록
ord-f7323dbcef384483968c17fe3f4b0f01
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091342B2

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