1-Hexene → HCID 86736255, compound

HRID 2163743Notes

Reaction equation

HRID 2163743 reaction equation
[CH3:1][CH:2]1[CH:7]([CH3:8])[CH:6]2[CH2:9][CH:3]1[CH:4]=[CH:5]2.[CH2:10]=[CH:11][CH2:12][CH2:13][CH2:14][CH3:15].[I-].C([Al+]CC)C>C1C=CC=CC=1>[CH3:1][CH:2]1[CH:7]([CH3:8])[CH:6]2[CH2:9][CH:3]1[CH:4]=[CH:5]2.[CH2:10]=[CH:11][CH2:12][CH2:13][CH2:14][CH3:15]

Participants

5

Reactant 3

HCID 115971-HexeneHCID 13652382HCID 13652382, compoundHCID 16686130AlEt2I

Product 1

HCID 86736255HCID 86736255, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-1606c97b75ce4ca2a8ec155f6536a026
Source dataset
uspto-grants-1979_01
Patent number
US04136247

Reaction notes

Loading…