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

HRID 1975895ノート

反応式

HRID 1975895 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[CH2:32][CH2:31][CH:28]([CH:29]=[CH:30]1)[CH2:27][CH:26]2[C:33]([O:35][CH2:36][CH2:37][CH2:38][OH:39])=[O:34].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[CH2:32][CH2:31][CH:28]([CH:29]=[CH:30]1)[CH2:27][CH:26]2[C:33]([O:35][CH2:36][CH2:37][CH2:38][OH:39])=[O:34]

参加物

6

反応物 4

HCID 6547AzobisisobutyronitrileHCID 14671028Ethyl maleimideHCID 18413667t-Butyl bicyclo[2,2,2]oct-5-ene-2-carboxylateHCID 229870623-Hydroxypropyl bicyclo[2,2,2]oct-5-ene-2-carboxylate

生成物 1

HCID 131722531Ethyl maleimide t-butyl bicyclo[2,2,2]oct-5-ene-2-carboxylate 3-hydroxypropyl bicyclo[2,2,2]oct-5-ene-2-carboxylate収率 75%

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 bicyclo[2,2,2]oct-5-ene-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/bicyclo[2,2,2]oct-5-ene-2-carboxylate) polymer was obtained at a yield of 75%

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 75%

出典と根拠

ORDレコード
ord-562ac457a4964c3aac994e6d27e8b4d6
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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