反応 #9852

ord-6126e02d02c2469fb6ad8fa1a7eee34a

反応方程式

O=c1n(O)c(=O)n(O)c(=O)n1O
hexahydro-1,3,5-trihydroxy-1,3,5-triazine-2,4,6-trione
Cc1ccc(C)cc1
p-xylene
O
water
Cc1ccc(C)cc1
p-xylene
CC(=O)O
acetic acid
O=C(O)c1ccc(C(=O)O)cc1
terephthalic acid
収率 99.0%

反応条件

温度
150°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONThe autoclave was charged with 2 MPa of air
  2. 2
    その他placed in a heated oil bath
  3. 3
    その他After the completion of reaction
  4. 4
    温度to cool down the reaction mixture quickly

実験手順

In an autoclave, 0.212 g of p-xylene, 0.011 g of hexahydro-1,3,5-trihydroxy-1,3,5-triazine-2,4,6-trione (3% by mole relative to p-xylene), 5 g of acetic acid, 0.003 g of cobalt(II) acetate.4H2O, 0.003 g of manganese(II) acetate.4H2O and 0.001 g of zirconium oxyacetate were placed. The autoclave was charged with 2 MPa of air and placed in a heated oil bath. The mixture was stirred at 150° C. for 12 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 high performance liquid chromatography and was found to yield terephthalic acid in 99% yield at 100% conversion of p-xylene.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091342B2uspto-grants-2006_08