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

HRID 1792992

反応式

HRID 1792992 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]>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

4

反応物 2

HCID 6961Pyromellitic AcidHCID 178418361HCID 178418361、化合物3 回

生成物 1

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

試薬・触媒・溶媒 1

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 of Rh supported on activated carbon (available from N.E. Chemcat Corporation) and 1656 g of water, and then the inner atmosphere was replaced with nitrogen gas while stirring the contents. Then, the inner atmosphere was replaced with hydrogen gas and the temperature was raised to 60° C. under a hydrogen pressure of 5.0 MPa. The reaction was continued for 2 h while maintaining the hydrogen pressure at 5.0 MPa. After replacing the hydrogen gas in the autoclave with nitrogen gas, the reaction product solution was taken out of the autoclave and filtered hot to separate the catalyst. The filtrate was concentrated under reduced pressure using a rotary evaporator to precipitate crystals. The precipitated crystals were subjected to solid-liquid separation and then dried to obtain 481 g of 1,2,4,5-cyclohexanetetracarboxylic acid (yield: 85.0%).

後処理

  1. filtrationfiltered hot
  2. customto separate the catalyst
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customa rotary evaporator
  5. customto precipitate crystals
  6. customThe precipitated crystals were subjected to solid-liquid separation
  7. customdried

出典と根拠

ORDレコード
ord-8279129301e5482eb7927fbcb8008844
出典データセット
uspto-grants-2006_07
特許番号
US07078477B2

関連ノート

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