Azobisisobutyronitrile → Di-tert-butyl 5-norbornene-2,3-dicarboxylate 2-hydroxyethyl 5-norbomene-2-carboxylate 5-norbomene-2,3-dicarboxylic acid maleic anhydride

HRID 1936531노트

반응식

HRID 1936531 반응식
[CH:1]12[CH2:7][CH:4]([CH:5]=[CH:6]1)[CH:3]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH:2]2[C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16].[CH:22]12[CH2:28][CH:25]([CH:26]=[CH:27]1)[CH2:24][CH:23]2[C:29]([O:31][CH2:32][CH2:33][OH:34])=[O:30].[CH:35]12[CH2:41][CH:38]([CH:39]=[CH:40]1)[CH:37]([C:42]([OH:44])=[O:43])[CH:36]2[C:45]([OH:47])=[O:46].[C:48]1(=[O:54])[O:53][C:51](=[O:52])[CH:50]=[CH:49]1.CC(N=NC(C#N)(C)C)(C#N)C>O1CCCC1>[CH:4]12[CH2:7][CH:1]([CH:6]=[CH:5]1)[CH:2]([C:15]([O:17][C:18]([CH3:19])([CH3:20])[CH3:21])=[O:16])[CH:3]2[C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9].[CH:22]12[CH2:28][CH:25]([CH:26]=[CH:27]1)[CH2:24][CH:23]2[C:29]([O:31][CH2:32][CH2:33][OH:34])=[O:30].[CH:35]12[CH2:41][CH:38]([CH:39]=[CH:40]1)[CH:37]([C:42]([OH:44])=[O:43])[CH:36]2[C:45]([OH:47])=[O:46].[C:51]1(=[O:52])[O:53][C:48](=[O:54])[CH:49]=[CH:50]1

참가 물질

7

반응물 5

HCID 6547AzobisisobutyronitrileHCID 7923Maleic AnhydrideHCID 979655-Norbornene-2,3-dicarboxylic acidHCID 120338232-Hydroxyethyl bicyclo[2.2.1]hept-5-ene-2-carboxylateHCID 219223175,6-Di(t-butoxycarbonyl)norbornene

생성물 1

HCID 131723220Di-tert-butyl 5-norbornene-2,3-dicarboxylate 2-hydroxyethyl 5-norbomene-2-carboxylate 5-norbomene-2,3-dicarboxylic acid maleic anhydride수율 31%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
67 °C

실험 절차

Di-tert-butyl 5-norbornene-2,3-dicarboxylate (0.85 mole), 2-hydroxyethyl 5-norbomene-2-carboxylate (0.1 mole), 5-norbornene-2,3-dicarboxylic acid (0.05 mole) and maleic anhydride (1 mole) were mixed together in tetrahydrofuran solvent, and AIBN (5.5 g) was added to the mixture as a polymerization initiator. Polymerization was performed under nitrogen atmosphere for 10 hours while maintaining the temperature at 67° C. When the polymerization was completed, the polymer was precipitated from ethyl ether and dried in vacuo to obtain pure poly(di-tert-butyl 5-norbornene-2,3-dicarboxylate/2-hydroxyethyl 5-norbomene-2-carboxylate/5-norbomene-2,3-dicarboxylic acid/maleic anhydride) of Chemical Formula 102 shown above (yield: 31%).

후처리

  1. customPolymerization
  2. customthe polymer was precipitated from ethyl ether
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-cfcd4e982b184ff0a6b8ca716104163c
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06391518B1

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