Azobisisobutyronitrile → Ethyl maleimide t-butyl bicyclo[2,2,2]oct-5-ene-2-carboxylate 3-hydroxypropyl 5-norbornene-2-carboxylate

HRID 1975891ノート

反応式

HRID 1975891 の反応式
[CH2:1]([C:3]1[C:4]([NH:6][C:7](=[O:9])[CH:8]=1)=[O:5])[CH3:2].[CH:10]12[CH2:17][CH2:16][CH:13]([CH:14]=[CH:15]1)[CH2:12][CH:11]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:3]1[C:4]([NH:6][C:7](=[O:9])[CH:8]=1)=[O:5])[CH3:2].[CH:10]12[CH2:17][CH2:16][CH:13]([CH:14]=[CH:15]1)[CH2:12][CH:11]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]

参加物

6

反応物 4

HCID 6547AzobisisobutyronitrileHCID 14671028Ethyl maleimideHCID 18413667t-Butyl bicyclo[2,2,2]oct-5-ene-2-carboxylateHCID 235020283-Hydroxypropyl 5-norbomene-2-carboxylate

生成物 1

HCID 86756649Ethyl maleimide t-butyl bicyclo[2,2,2]oct-5-ene-2-carboxylate 3-hydroxypropyl 5-norbornene-2-carboxylate収率 83%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl maleimide (1 mol.), t-butyl bicyclo[2,2,2]oct-5-ene-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) was added thereto, and the resulting solution was reacted at a temperature between 60° C. and 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(ethyl maleimide/t-butyl bicyclo[2,2,2]oct-5-ene-2-carboxylate/3-hydroxypropyl 5-norbornene-2-carboxylate) polymer was obtained at a yield of about 83%. NMR spectra of the polymer is illustrated in FIG. 4.

後処理

  1. customthe resulting solution was reacted at a temperature between 60° C. and 70° C. in a nitrogen atmosphere for 10 hours
  2. customAfter a high molecular weight was achieved by the reaction
  3. customthe resultant product was precipitated in an ethyl ether or hexane solvent
  4. customThe gathered precipitate was dried
  5. customwas obtained at a yield of about 83%

出典と根拠

ORDレコード
ord-8075e20c3660497d8f10866387ef1c38
出典データセット
uspto-grants-2001_05
特許番号
US06225020B1

反応ノート

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