Réaction #324365

Équation de réaction

hydrogen

pyromellitic acid

hydrogen

hydrogen

hydrogen

→

1,2,4,5-cyclohexanetetracarboxylic acid

Rendement 85.1%

Solvants

water

Conditions de réaction

Traitement

1. 1
   Filtrationwas filtered while it
2. 2
   Autreto separate the catalyst
3. 3
   ConcentrationThe filtrate was concentrated
4. 4
   Autreby evaporating water under reduced pressure
5. 5
   Autrea rotary evaporator
6. 6
   Autreto precipitate crystals
7. 7
   AutreThe precipitated crystals were separated by solid-liquid separation at room temperature
8. 8
   Autredried

Mode opératoire

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%).

Source