1-Butene → Norbornene 1-Butene

500 ml dry benzene cosolvent, 77 ml 2-norbornene solution, 10 ml of the 1-butene solution, and 6 ml of the diethylaluminum iodide solution were charged to a dry, nitrogen-purged quart bottle. 7.5 ml of the MoCl5 solution was charged last, and the bottle was shaken. Polymerization occurred so rapidly that the reaction was terminated after 7-8 minutes using a mixture of 1.5 ml ethanolamine, 10 ml of an antioxidant solution (10 grams of 2,2',2"-tris[3(3,5-di-t-butyl-4-hydroxyphenyl) propionyloxy] ethyl isocyanurate in 100 ml benzene) and 1 ml ethanol. The polymer cement was allowed to stand for about 12 hours and coagulated using excess Solution A in a Waring blender. A slightly yellow solid formed and was filtered and vacuum dried at 60° C. The solid weighed 57.4 grams after drying. It was a ring-opened 2-norbornene/1-butene copolymer having a DSV of about 2.3.

1. custompurged quart bottle
2. addition7.5 ml of the MoCl5 solution was charged last
3. customPolymerization
4. customwas terminated after 7-8 minutes
5. additiona mixture of 1.5 ml ethanolamine, 10 ml of an antioxidant solution (10 grams of 2,2',2"-tris[3(3,5-di-t-butyl-4-hydroxyphenyl) propionyloxy] ethyl isocyanurate in 100 ml benzene) and 1 ml ethanol
6. customA slightly yellow solid formed
7. filtrationwas filtered
8. customvacuum dried at 60° C
9. customafter drying

ORD record

ord-5761063912194cd2af00e6a1c6c2c493

Source dataset

uspto-grants-1979_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04136248