Pyromellitic Acid → 1,2,4,5-Cyclohexanetetracarboxylic Acid

HRID 1351049노트

반응식

HRID 1351049 반응식
[C:1]([OH:18])(=[O:17])[C:2]1[C:3](=[CH:7][C:8](=[C:12]([CH:16]=1)[C:13]([OH:15])=[O:14])[C:9]([OH:11])=[O:10])[C:4]([OH:6])=[O:5].[H][H]>[Rh].O>[CH:8]1([C:9]([OH:11])=[O:10])[CH2:7][CH:3]([C:4]([OH:6])=[O:5])[CH:2]([C:1]([OH:18])=[O:17])[CH2:16][CH:12]1[C:13]([OH:15])=[O:14]

참가 물질

5

반응물 2

HCID 6961Pyromellitic AcidHCID 178418361HCID 178418361, 화합물3회

생성물 1

HCID 28349461,2,4,5-Cyclohexanetetracarboxylic Acid수율 85.1%

시약·촉매·용매 2

HCID 23948Rhodium촉매HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

A 5-L Hastelloy (H22) autoclave was charged with 552 g of pyromellitic acid, 200 g of a catalyst, rhodium carried on activated carbon, available from N.E. Chemcat Corporation, and 1656 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 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 h. Then, after replacing the hydrogen gas 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 and dried to obtain 481 g of 1,2,4,5-cyclohexanetetracarboxylic acid (yield: 85.0%).

후처리

  1. filtrationwas filtered while it
  2. customto separate the catalyst
  3. concentrationThe filtrate was concentrated
  4. customby evaporating water under reduced pressure
  5. customa rotary evaporator
  6. customto precipitate crystals
  7. customThe precipitated crystals were separated by solid-liquid separation
  8. customdried

출처 및 근거

ORD 기록
ord-add9ba84556949f59ee32ff80c0ca223
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217462B2

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