反応 #324365

ord-8ddcf2cd89834c66bb4be89b8a8530c1

反応方程式

[H][H]
hydrogen
O=C(O)c1cc(C(=O)O)c(C(=O)O)cc1C(=O)O
pyromellitic acid
[H][H]
hydrogen
[H][H]
hydrogen
[H][H]
hydrogen
O=C(O)C1CC(C(=O)O)C(C(=O)O)CC1C(=O)O
1,2,4,5-cyclohexanetetracarboxylic acid
収率 85.1%

溶媒

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過was filtered while it
  2. 2
    その他to separate the catalyst
  3. 3
    濃縮The filtrate was concentrated
  4. 4
    その他by evaporating water under reduced pressure
  5. 5
    その他a rotary evaporator
  6. 6
    その他to precipitate crystals
  7. 7
    その他The precipitated crystals were separated by solid-liquid separation at room temperature
  8. 8
    その他dried

実験手順

A 5-L Hastelloy (HC22) autoclave was charged with 552 g of pyromellitic acid, 200 g of a catalyst, that is, rhodium carried on activated carbon, available from N.E. Chemcat Corporation, and 1,656 g of water. The inner atmosphere of the reactor was replaced with nitrogen gas under stirring. After replacing the inner atmosphere of the reactor with hydrogen gas, the hydrogen pressure in the reactor was adjusted to 5.0 MPa and the temperature was raised to 60° C. While maintaining the hydrogen pressure at 5.0 MPa, the reaction was allowed to proceed for 2 hours. Then, after replacing the hydrogen gas in the reactor with nitrogen gas, the reaction product solution taken out of the autoclave was filtered while it was still hot to separate the catalyst. The filtrate was concentrated by evaporating water under reduced pressure using a rotary evaporator to precipitate crystals. The precipitated crystals were separated by solid-liquid separation at room temperature and dried, thereby obtaining 481 g of 1,2,4,5-cyclohexanetetracarboxylic acid (yield: 85.0%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08642181B2uspto-grants-2014_02