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

HRID 237183

反応式

HRID 237183 の反応式
[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]

参加物

5

反応物 2

HCID 6961Pyromellitic AcidHCID 178418361HCID 178418361、化合物4 回

生成物 1

HCID 28349461,2,4,5-Cyclohexanetetracarboxylic Acid収率 85.1%

試薬・触媒・溶媒 2

HCID 23948Rhodium触媒HCID 962Water溶媒

反応条件

温度
60 °C

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%).

後処理

  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 at room temperature
  8. customdried

出典と根拠

ORDレコード
ord-8ddcf2cd89834c66bb4be89b8a8530c1
出典データセット
uspto-grants-2014_02
特許番号
US08642181B2

関連ノート

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