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

HRID 237184

반응식

HRID 237184 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

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%).

후처리

  1. customequipped with a Dimroth condenser
  2. temperatureThe temperature was raised to the refluxing temperature of the solvent under a nitrogen gas atmosphere
  3. temperatureto reflux for 10 min
  4. customwas decreased 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-91fc894e31404015bb7dee5482d03332
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642181B2

연결된 노트

불러오는 중…