反応 #2063071

ord-43a23beb0e4e480a8b474e2599a4b5d1

反応方程式

CC(C)(C#N)N=NC(C)(C)C#N
2,2′-azobisisobutyronitrile
CCCC1=CC(=O)NC1=O
Propyl maleimide
CC(C)(C)OC(=O)C1CC2C=CC1C2
t-butyl 5-norbornene-2-carboxylate
O=C(OCCCO)C1CC2C=CC1C2
3-hydroxypropyl 5-norbornene-2-carboxylate
CC(C)(C)OC(=O)C1CC2C=CC1C2.CCCC1=CC(=O)NC1=O.O=C(OCCCO)C1CC2C=CC1C2
propyl maleimide t-butyl 5-norbornene-2-carboxylate 3-hydroxypropyl 5-norbornene-2-carboxylate
収率 82.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他After a high molecular weight was achieved by the reaction
  2. 2
    その他the resultant product was precipitated in an ethyl ether or hexane solvent
  3. 3
    その他The gathered precipitate was dried
  4. 4
    その他was obtained at a yield of about 82%

実験手順

Propyl maleimide (1 mol.), t-butyl 5-norbornene-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) were added thereto, then the resultant solution was reacted at a temperature of 60° C. to 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(propyl maleimide/t-butyl 5-norbornene-2-carboxylate/3-hydroxypropyl 5-norbornene-2-carboxylate) polymer was obtained at a yield of about 82%. NMR spectra of the polymer is illustrated in FIG. 3.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06225020B1uspto-grants-2001_05