반응 #324365

ord-8ddcf2cd89834c66bb4be89b8a8530c1

반응 방정식

[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
수율 85.1%

용매

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과was filtered while it
  2. 2
    기타to separate the catalyst
  3. 3
    농축The filtrate was concentrated
  4. 4
    기타by evaporating water under reduced pressure
  5. 5
    기타a rotary evaporator
  6. 6
    기타to precipitate crystals
  7. 7
    기타The precipitated crystals were separated by solid-liquid separation at room temperature
  8. 8
    기타dried

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08642181B2uspto-grants-2014_02