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

HRID 429011ノート

反応式

HRID 429011 の反応式
[C:1]1(=[O:7])[O:6][C:4](=[O:5])[CH:3]=[CH:2]1.[CH:8]12[CH2:15][CH2:14][CH:11]([CH:12]=[CH:13]1)[CH2:10][CH:9]2[C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17].N(C(C)(C)C#N)=NC(C)(C)C#N>O1CCCC1>[C:4]1(=[O:5])[O:6][C:1](=[O:7])[CH:2]=[CH:3]1.[CH:8]12[CH2:15][CH2:14][CH:11]([CH:12]=[CH:13]1)[CH2:10][CH:9]2[C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17].[CH:8]12[CH2:13][CH:11]([CH:14]=[CH:15]1)[CH2:10][CH:9]2[C:16]([O:18][CH2:19][CH2:22][CH2:4][OH:5])=[O:17]

参加物

5

反応物 3

HCID 6547AzobisisobutyronitrileHCID 7923Maleic AnhydrideHCID 18413667t-Butyl bicyclo[2,2,2]oct-5-ene-2-carboxylate

生成物 1

HCID 86757578Maleic anhydride t-butyl bicyclo[2,2,2]oct-5-ene-2-carboxylate 3-hydroxypropyl 5-norbornene-2-carboxylate収率 50%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Maleic anhydride (1 mol.), t-butyl bicyclo[2,2,2]oct-5-ene-2-carboxylate (0.5 mol.), and 3-hydroxy propyl 5-norbornene-2-carboxylate (0.5 mol.) were dissolved in 200 gms of tetrahydrofuran (THF), 6 gms of 2,2′-azobisisobutyronitrile (AIBN) was added thereto, and then the resultant solution was reacted at a temperature of 67° C. in a nitrogen atmosphere for 10 hours. After a high molecule weight was achieved by the reaction, the resultant product was precipitated in an ethyl ether solvent. The gathered precipitate was dried, and 150 gms of the desirable poly(maleic anhydride/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 50%. NMR spectra of the polymer is illustrated in FIG. 5.

後処理

  1. customAfter a high molecule weight was achieved by the reaction
  2. customthe resultant product was precipitated in an ethyl ether solvent
  3. customThe gathered precipitate was dried

出典と根拠

ORDレコード
ord-cf7fa89251d3477eb64d7e31765bd6fd
出典データセット
uspto-grants-2001_11
特許番号
US06316162B1

反応ノート

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