Azobisisobutyronitrile → Bicyclo[2.2.1]hept-5-ene-2-methanol bicyclo[2.2.1]hept-5-ene-2-carboxylic acid norbornene maleic anhydride

HRID 986895

反応式

HRID 986895 の反応式
[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH:3]=[CH:2]2.[CH:8]12[CH2:14][CH:11]([CH:12]=[CH:13]1)[CH2:10][CH:9]2[CH2:15][OH:16].[CH:17]12[CH2:23][CH:20]([CH:21]=[CH:22]1)[CH2:19][CH:18]2[C:24]([OH:26])=[O:25].[C:27]1(=[O:33])[O:32][C:30](=[O:31])[CH:29]=[CH:28]1.CC(N=NC(C#N)(C)C)(C#N)C>O1CCCC1>[CH:8]12[CH2:14][CH:11]([CH:12]=[CH:13]1)[CH2:10][CH:9]2[CH2:15][OH:16].[CH:17]12[CH2:23][CH:20]([CH:21]=[CH:22]1)[CH2:19][CH:18]2[C:24]([OH:26])=[O:25].[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH:3]=[CH:2]2.[C:30]1(=[O:31])[O:32][C:27](=[O:33])[CH:28]=[CH:29]1

参加物

7

反応物 5

HCID 6547AzobisisobutyronitrileHCID 7923Maleic AnhydrideHCID 103522-NorborneneHCID 78946Bicyclo(2.2.1)hept-5-ene-2-methanolHCID 789495-Norbornene-2-carboxylic acid

生成物 1

HCID 86759191Bicyclo[2.2.1]hept-5-ene-2-methanol bicyclo[2.2.1]hept-5-ene-2-carboxylic acid norbornene maleic anhydride

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 70 ml of tetrahydrofuran was added 0.04 M of norbornylene, 0.1 M of bicyclo[2.2.1]hept-5-ene-2-methanol, 0.06 M of bicyclo[2.2.1]hept-5-ene-2-carboxylic acid, 0.2 M of maleic anhydride and 0.4 g of AIBN. The resulting solution was reacted at 67° C. for 8 hours. Thereafter, a polymer was precipitated and filtered in petroleum ether/ether (1/1) solution, to obtain the title polymer. Here, the polymer was washed with aqueous Na2CO3 solution (5%), and re-washed with distilled water to completely remove base. The resulting resin was vacuum-dried to obtain a pure resin (yield: 51%).

後処理

  1. customThe resulting solution was reacted at 67° C. for 8 hours
  2. customThereafter, a polymer was precipitated
  3. filtrationfiltered in petroleum ether/ether (1/1) solution

出典と根拠

ORDレコード
ord-3da923555ce94d79bc6c6fa0db87a994
出典データセット
uspto-grants-2003_10
特許番号
US06630281B2

関連ノート

読み込み中…