Acetic Anhydride → 1,2,4,5-Cyclohexanetetracarboxylic dianhydride

HRID 1351050노트

반응식

HRID 1351050 반응식
[CH:1]1([C:16]([OH:18])=[O:17])[CH2:6][CH:5]([C:7]([OH:9])=O)[CH:4]([C:10]([OH:12])=[O:11])[CH2:3][CH:2]1[C:13]([OH:15])=O.C(OC(=O)C)(=O)C>>[CH2:6]1[CH:1]2[C:16]([O:18][C:13](=[O:15])[CH:2]2[CH2:3][CH:4]2[C:10]([O:11][C:7](=[O:9])[CH:5]12)=[O:12])=[O:17]

참가 물질

3

반응물 2

HCID 7918Acetic AnhydrideHCID 28349461,2,4,5-Cyclohexanetetracarboxylic Acid

생성물 1

HCID 144536671,2,4,5-Cyclohexanetetracarboxylic dianhydride수율 96.7%

실험 절차

Successively, 450 g of the obtained 1,2,4,5-cyclohexanetetracarboxylic acid and 4000 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 to allow the solvent to reflux for 10 min. Thereafter, the temperature was lowered 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 anhydration: 96.6%).

후처리

  1. customequipped with a Dimroth condenser
  2. temperatureThe temperature was raised to the refluxing temperature of the solvent
  3. temperatureto reflux for 10 min
  4. customwas lowered to room temperature
  5. stirringunder stirring
  6. customto precipitate crystals
  7. customThe precipitated crystals were separated by solid-liquid separation
  8. customdried
  9. customto obtain primary crystals
  10. customThe mother liquor after separation
  11. concentrationwas concentrated under reduced pressure
  12. customa rotary evaporator
  13. customto precipitate crystals
  14. customThe precipitated crystals were separated by solid-liquid separation
  15. customdried
  16. customto obtain secondary crystals

출처 및 근거

ORD 기록
ord-655576fbb6d94198a20f67c3dca300f0
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217462B2

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