Reaktion #324366

Reaktionsgleichung

1,2,4,5-cyclohexanetetracarboxylic acid

acetic anhydride

→

1,2,4,5-cyclohexanetetracarboxylic dianhydride

Ausbeute 96.7%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeequipped with a Dimroth condenser
2. 2
   TemperaturThe temperature was raised to the refluxing temperature of the solvent under a nitrogen gas atmosphere
3. 3
   Temperaturto reflux for 10 min
4. 4
   Sonstigewas decreased to room temperature
5. 5
   workup.STIRRINGunder stirring
6. 6
   Sonstigeto precipitate crystals
7. 7
   SonstigeThe precipitated crystals were separated by solid-liquid separation
8. 8
   Sonstigedried
9. 9
   Sonstigeto obtain primary crystals
10. 10
    SonstigeThe mother liquor after separation
11. 11
    Einengenwas concentrated under reduced pressure
12. 12
    Sonstigea rotary evaporator
13. 13
    Sonstigeto precipitate crystals
14. 14
    SonstigeThe precipitated crystals were separated by solid-liquid separation
15. 15
    Sonstigedried
16. 16
    Sonstigeto obtain secondary crystals

Vorschrift

Subsequently, 450 g of the obtained 1,2,4,5-cyclohexanetetracarboxylic acid and 4,000 g of acetic anhydride were charged into a 5-L glass separable flask equipped with a Dimroth condenser. The inner atmosphere of the reactor was replaced with nitrogen gas under stirring. The temperature was raised to the refluxing temperature of the solvent under a nitrogen gas atmosphere to allow the solvent to reflux for 10 min. After that, the temperature was decreased to room temperature under stirring to precipitate crystals. The precipitated crystals were separated by solid-liquid separation and dried to obtain primary crystals. The mother liquor after separation was concentrated under reduced pressure using a rotary evaporator to precipitate crystals. The precipitated crystals were separated by solid-liquid separation and dried to obtain secondary crystals. In total of the primary and secondary crystals, 375 g of 1,2,4,5-cyclohexanetetracarboxylic dianhydride was obtained (yield of the dianhydride: 96.6%).

Quelle