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

HRID 1443023

反応式

HRID 1443023 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4 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 autoclave made of Hastelloy (HC22) was charged with 552 g of pyromellitic acid, 200 g of a catalyst formed by supporting Rh on activated carbon (available from N.E. Chemcat Corporation) and 1656 g of water. The interior of the autoclave was replaced with a hydrogen gas while stirring the contents. Then, 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. After replacing the hydrogen gas in the autoclave with nitrogen gas, the reaction product solution was discharged from the autoclave. The reaction product solution was filtered while it was hot to separate the catalyst. The filtrate was concentrated by distillation under reduced pressure using a rotary evaporator to evaporate off water, thereby precipitating crystals. The precipitated crystals were collected by a solid-liquid separation at room temperature, and then, dried to obtain 481 g of 1,2,4,5-cyclohexanetetracarboxylic acid (yield: 85.0%).

後処理

  1. customformed
  2. filtrationThe reaction product solution was filtered while it
  3. customto separate the catalyst
  4. concentrationThe filtrate was concentrated by distillation under reduced pressure
  5. customa rotary evaporator
  6. customto evaporate off water
  7. customprecipitating crystals
  8. customThe precipitated crystals were collected by a solid-liquid separation at room temperature
  9. customdried

出典と根拠

ORDレコード
ord-ad466644a87a442ab26ac0104f593a99
出典データセット
uspto-grants-2010_02
特許番号
US07659360B2

関連ノート

読み込み中…