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Azobisisobutyronitrile → Propyl maleimide t-butyl 5-norbornene-2-carboxylate 3-hydroxypropyl 5-norbornene-2-carboxylate

HRID 1975889
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HRID 1975889 반응식
[CH2:1]([C:4]1[C:5]([NH:7][C:8](=[O:10])[CH:9]=1)=[O:6])[CH2:2][CH3:3].[CH:11]12[CH2:17][CH:14]([CH:15]=[CH:16]1)[CH2:13][CH:12]2[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19].[CH:25]12[CH2:31][CH:28]([CH:29]=[CH:30]1)[CH2:27][CH:26]2[C:32]([O:34][CH2:35][CH2:36][CH2:37][OH:38])=[O:33].N(C(C)(C)C#N)=NC(C)(C)C#N>O1CCCC1>[CH2:1]([C:4]1[C:5]([NH:7][C:8](=[O:10])[CH:9]=1)=[O:6])[CH2:2][CH3:3].[CH:11]12[CH2:17][CH:14]([CH:15]=[CH:16]1)[CH2:13][CH:12]2[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19].[CH:25]12[CH2:31][CH:28]([CH:29]=[CH:30]1)[CH2:27][CH:26]2[C:32]([O:34][CH2:35][CH2:36][CH2:37][OH:38])=[O:33]
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참가 물질

6

반응물 4

HCID 6547AzobisisobutyronitrileHCID 15607334Bicyclo[2.2.1]hept-5-ene-2-carboxylic acid, 1,1-dimethylethyl esterHCID 21880478Propyl maleimideHCID 235020283-Hydroxypropyl 5-norbomene-2-carboxylate

생성물 1

HCID 86756647Propyl maleimide t-butyl 5-norbornene-2-carboxylate 3-hydroxypropyl 5-norbornene-2-carboxylate수율 82%

시약·촉매·용매

1
HCID 8028Tetrahydrofuran용매

실험 절차

Propyl maleimide (1 mol.), t-butyl 5-norbornene-2-carboxylate (0.5 mol.), and 3-hydroxypropyl 5-norbornene-2-carboxylate (0.5 mol.) were dissolved in 50 g to 300 g of tetrahydrofuran (THF), 2 g to 15 g of 2,2′-azobisisobutyronitrile (AIBN) were added thereto, then the resultant solution was reacted at a temperature of 60° C. to 70° C. in a nitrogen atmosphere for 10 hours. After a high molecular weight was achieved by the reaction, the resultant product was precipitated in an ethyl ether or hexane solvent. The gathered precipitate was dried, and the desired poly(propyl maleimide/t-butyl 5-norbornene-2-carboxylate/3-hydroxypropyl 5-norbornene-2-carboxylate) polymer was obtained at a yield of about 82%. NMR spectra of the polymer is illustrated in FIG. 3.

후처리

  1. customAfter a high molecular weight was achieved by the reaction
  2. customthe resultant product was precipitated in an ethyl ether or hexane solvent
  3. customThe gathered precipitate was dried
  4. customwas obtained at a yield of about 82%

출처 및 근거

ORD 기록
ord-43a23beb0e4e480a8b474e2599a4b5d1
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06225020B1

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