反应详情

50 ml dry benzene cosolvent, 7 ml 5,6-dimethyl-2-norbornene, 0.5 ml of the 1-hexene solution, and 0.6 ml of the diethylaluminum iodide solution were charged to a dry, nitrogen-purged 7 oz. bottle. 0.75 ml of the MoCl5 solution was charged last, and the bottle was shaken. After 1 hour the reaction was shortstopped using a mixture of 0.1 ml ethanolamine and 2 ml Solution A. 1 ml of an antioxidant solution was also added (0.1 g/ml of 2,2'-methylenebis-[4-methyl-6-t-butylphenol] in benzene). The polymer cement was coagulated with excess Solution A in a Waring blender. About 5.8 grams of a 5,6-dimethyl-2-norbornene/1-hexene copolymer was recovered after filtration and vacuum drying at 60° C. The copolymer was a solid with a DSV (as defined heretofore) of about 1.59.

1. custompurged 7 oz. bottle
2. addition0.75 ml of the MoCl5 solution was charged last
3. additiona mixture of 0.1 ml ethanolamine and 2 ml Solution A
4. addition1 ml of an antioxidant solution was also added (0.1 g/ml of 2,2'-methylenebis-[4-methyl-6-t-butylphenol] in benzene)
5. customAbout 5.8 grams of a 5,6-dimethyl-2-norbornene/1-hexene copolymer was recovered
6. filtrationafter filtration and vacuum
7. customdrying at 60° C