Acetic Acid → P-Toluic Acid

HRID 9740

反応式

HRID 9740 の反応式
[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].ON1C(=O)N(O)C(=O)N(O)C1=O.O=O>[Ti].C([O-])(=O)C.[Co+2].C([O-])(=O)C.C([O-])(=O)C.[Mn+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

参加物

10

反応物 4

HCID 176Acetic AcidHCID 977OxygenHCID 7470P-Toluic AcidHCID 104197231,3,5-Trihydroxy-1,3,5-triazinane-2,4,6-trione

生成物 2

HCID 7470P-Toluic AcidHCID 7489Terephthalic Acid

試薬・触媒・溶媒 4

HCID 6277Cobalt diacetate触媒HCID 12525Manganous Acetate触媒HCID 23963Titanium触媒HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

In a 500-ml titanium autoclave equipped with a stirrer and a pressure gauge, 15.36 g of p-toluic acid, 104.0 g of acetic acid, 0.066 g of hexahydro-1,3,5-trihydroxy-1,3,5-triazine-2,4,6-trione (1,3,5-trihydroxyisocyanuric acid) (0.33% by mole relative to p-toluic acid), 0.112 g of cobalt(II) acetate.4H2O and 0.277 g of manganese(II) acetate.4H2O 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 63% yield at 68% conversion of p-toluic acid.

後処理

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

出典と根拠

ORDレコード
ord-bd8297b3cf7f4124a97a04ca91aa86e8
出典データセット
uspto-grants-2006_08
特許番号
US07091342B2

関連ノート

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