Ethanolamine → HCID 86644225, compound

A 2/1 molar ratio of 1,2-dihydrodicyclopentadiene (DHDCPD) to 2-norbornene was used as follows to prepare the first DHDCPD/2-norbornene/1-hexene copolymer of example 1. 500 ml dry toluene cosolvent, 23.1 ml of a 2-norbornene solution (89.2 wt.% in toluene), 55.4 ml DHDCPD, 9 ml of the 1-hexene 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 with shaking. Polymerization occurred rapidly, and after 1 hour the reaction was shortstopped using a mixture of 1 ml ethanolamine, 3 ml Solution A, and 6 ml of an antioxidant solution (0.1 g/ml of Ethyl 330 in toluene; Ethyl 330 is 1,3,5-trimethyl-2,4,6-tris[3,5-di-t-butyl-2-hydroxybenzyl]benzene). The polymer cement was washed twice with 2 liters of water per wash. Each water wash was discarded. An additional 6 ml of the antioxidant solution was added to the washed cement, which then was coagulated using excess Solution A in a Waring blender. A solid, ring-opened DHDCPD/2-norbornene/1-hexene copolymer was recovered by filtering and vacuum drying and found to have a DSV (as defined heretofore) of about 1.41.

1. custompurged quart bottle
2. addition7.5 ml of the MoCl5 solution was charged last
3. customPolymerization
4. washThe polymer cement was washed twice with 2 liters of water
5. washper wash
6. washEach water wash
7. additionAn additional 6 ml of the antioxidant solution was added to the washed cement, which
8. customA solid, ring-opened DHDCPD/2-norbornene/1-hexene copolymer was recovered
9. filtrationby filtering
10. customvacuum drying

ORD record

ord-856cb5f75f474750a71bd7ee6c78e5ef

Source dataset

uspto-grants-1979_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04136249