反応 #2383778

ord-1047302d657c4c47b2d228796d2cf922

反応方程式

C1CCOC1
tetrahydrofuran
O=C1C=CC(=O)O1
maleic anhydride
C=C1CC2C=CC1C2.O=C1C=CC(=O)O1
5-methylenebicyclo[2.2.1]hept-2-ene maleic anhydride
収率 183.7%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他equipped with a thermometer, a condenser pipe, and a nitrogen inlet pipe
  2. 2
    温度the mixture was heated
  3. 3
    温度under reflux at 70 C
  4. 4
    workup.ADDITIONwhile introducing nitrogen for 8 hr
  5. 5
    その他polymerization
  6. 6
    その他After the completion of the polymerization
  7. 7
    その他to precipitate the resultant polymer, which
  8. 8
    その他was then dried

実験手順

This synthesis example is directed to the synthesis of polymer (1b) (illustrated below as chemical formulas 14 or 15), a γ-hydroxy carboxylic acid structure. 21.2 g of 5-ethylenebicyclo[2.2.1]hept-2-ene, 19.6 g of maleic anhydride, 2.56 g of 2,2′-azobisisobutyronitrile, and 240 g of tetrahydrofuran were placed in a 500-ml, three-necked flask equipped with a thermometer, a condenser pipe, and a nitrogen inlet pipe, and the mixture was heated under reflux at 70 C. while introducing nitrogen for 8 hr to conduct polymerization. After the completion of the polymerization, the reaction mixture was poured into 1000 ml of n-hexane to precipitate the resultant polymer, which was then dried to give 37.5 g of a 5-methylenebicyclo[2.2.1]hept-2-ene/maleic anhydride copolymer (1a) (yield 92%). The polymer was analyzed by various methods and was found to mainly have a structure represented by the following formula:

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06489082B1uspto-grants-2002_12