Reacción #324365

Ecuación de reacción

hydrogen

pyromellitic acid

hydrogen

hydrogen

hydrogen

→

1,2,4,5-cyclohexanetetracarboxylic acid

Rendimiento 85.1%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Filtraciónwas filtered while it
2. 2
   Otroto separate the catalyst
3. 3
   ConcentraciónThe filtrate was concentrated
4. 4
   Otroby evaporating water under reduced pressure
5. 5
   Otroa rotary evaporator
6. 6
   Otroto precipitate crystals
7. 7
   OtroThe precipitated crystals were separated by solid-liquid separation at room temperature
8. 8
   Otrodried

Procedimiento

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%).

Fuente