تفاعل #1106653

ord-73cee0248ebe481396b5548784831e09

معادلة التفاعل

O=C1C=CC(=O)O1
Maleic Anhydride
C1=CC2CCC1C2
2-Norbornene
CC(C)(C#N)N=NC(C)(C)C#N
AIBN
C1=CC2CCC1C2.O=C1C=CC(=O)O1
MA NB
المردود 90.2%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONcharged to an appropriately sized reaction vessel
  2. 2
    أخرىThe solution was sparged with nitrogen for 10 min
  3. 3
    أخرىto remove oxygen
  4. 4
    درجة الحرارةafter which the solution was cooled to room temperature
  5. 5
    workup.ADDITIONThe reaction mixture was then diluted with 2.0 g of THF
  6. 6
    workup.ADDITIONwas added to hexane (1 L)
  7. 7
    أخرىto give a white powder that
  8. 8
    ترشيحwas filtered
  9. 9
    أخرىdried in a vacuum oven at 80° C. for 16 hr

الإجراء التجريبي

Maleic Anhydride (MA, 7.4 g, 75.0 mmol), 2-Norbornene (NB, 7.1 g, 75.0 mmol) and AIBN (1.2 g, 7.5 mmol) was dissolved in THF (20.4 g) and charged to an appropriately sized reaction vessel. The solution was sparged with nitrogen for 10 min to remove oxygen and then heated to 70° C. The mixture was allowed to stir at 70° C. for 5.0 hr, after which the solution was cooled to room temperature. The reaction mixture was then diluted with 2.0 g of THF and was added to hexane (1 L) to give a white powder that was filtered and dried in a vacuum oven at 80° C. for 16 hr. Approximately, 13.0 g (90%) of the MA/NB polymer was isolated (GPC Mw=4,100 Mn=1,800).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08715900B2uspto-grants-2014_05