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Acetic Acid → P-Toluic Acid

HRID 9741
ノート
印刷プレビュー

反応式

HRID 9741 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].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.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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 4

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

生成物 2

HCID 7470P-Toluic AcidHCID 7489Terephthalic Acid

試薬・触媒・溶媒 4

HCID 6277
Cobalt 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, 0.114 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.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 90% yield at 93% 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-3d5750931bd44381b0102746045a956c
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07091342B2

反応ノート

読み込み中…

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