Acetic Acid → P-Toluic Acid

HRID 1182328

반응식

HRID 1182328 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([OH:10])=[O:9])=[CH:6][CH:7]=1.[C:11]([OH:14])(=[O:13])[CH3:12].C(ON1C(=O)N(OC(=O)C)C(=O)N(OC(=O)C)C1=O)(=O)C.O=O>[Ti].C([O-])(=O)C.[Co+2].C([O-])(=O)C.O>[C:8]([OH:10])(=[O:9])[C:5]1[CH:6]=[CH:7][C:12]([C:11]([OH:14])=[O:13])=[CH:3][CH:4]=1.[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([OH:10])=[O:9])=[CH:6][CH:7]=1

참가 물질

9

반응물 4

HCID 176Acetic AcidHCID 977OxygenHCID 7470P-Toluic AcidHCID 113011241,3,5-Triacetoxy-hexahydro-1,3,5-triazine-2,4,6-trione

생성물 2

HCID 7470P-Toluic AcidHCID 7489Terephthalic Acid

시약·촉매·용매 3

HCID 6277Cobalt diacetate촉매2회HCID 23963Titanium촉매HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

In a 500-ml titanium autoclave equipped with a stirrer and a pressure gauge, 15.36 g of p-toluicacid, 104.0 g of acetic acid, 0.114 g of 1,3,5-triacetoxy-hexahydro-1,3,5-triazine-2,4,6-trione (1,3,5-triacetoxyisocyanuric acid) (0.33% by mole relative to p-toluic acid), 0.112 g of cobalt (II) acetate 4 H2O and 0.277 g of manganese(II) acetate 4 H2O were placed. The autoclave was charged with 2 MPa of oxygen gas and 2 MPa of nitrogen gas and placed in a heated oil bath. The mixture was stirred at 150° C. for 1 hour. After the completion of the reaction, the autoclave was placed on cold water to cool down the reaction mixture quickly. The resulting mixture was analyzed by high performance liquid chromatography and was found to yield terephthalic acid in 90% yield at 93% conversion of p-toluic acid.

후처리

  1. customplaced in a heated oil bath
  2. customAfter the completion of the reaction
  3. temperatureto cool down the reaction mixture quickly

출처 및 근거

ORD 기록
ord-abca0c6b5bbc43b08c2a87a32187104c
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07288649B2

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