Dicyclopentadiene → HCID 131711406, compound

HRID 2163753Notes

Reaction equation

HRID 2163753 reaction equation
[CH2:1]1[CH:5]2[CH:6]3[CH:10]=[CH:9][CH:8]([CH:4]2[CH:3]=[CH:2]1)[CH2:7]3.[CH2:11]=[CH:12][CH2:13][CH2:14][CH2:15][CH3:16].[I-].C([Al+]CC)C>C1C=CC=CC=1>[CH2:1]1[CH:5]2[CH:6]3[CH:10]=[CH:9][CH:8]([CH:4]2[CH:3]=[CH:2]1)[CH2:7]3.[CH2:11]=[CH:12][CH2:13][CH2:14][CH2:15][CH3:16]

Participants

5

Reactant 3

HCID 6492DicyclopentadieneHCID 115971-HexeneHCID 16686130AlEt2I

Product 1

HCID 131711406HCID 131711406, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

2500 ml dry benzene cosolvent, 360 ml dicyclopentadiene solution (90 wt.% in benzene), 85 ml of the 1-hexene solution, and 30 ml of the diethylaluminum iodide solution were charged to a dry, nitrogen-purged 1-gallon bottle. 37.5 ml of the MoCl5 solution was charged last, and the bottle was shaken. After 1 hour the reaction was shortstopped with 7.5 ml ethanolamine, 25 ml Solution A and 5 ml water. The reaction mixture was transferred to a beaker and 500 ml benzene added. The beaker contents were washed five times with 4,000 ml water per wash. The water was discarded after each wash. 3.1 grams of Ethyl 712 antioxidant (4,4'-bis[2,6-di-t-butylphenol]) was added after washing was complete. The polymer cement was vacuum dried at 77° C. for 8 hours. A solid, ring-opened dicyclopentadiene/1-hexene copolymer was recovered weighing 316 grams and having a DSV of about 1.36.

Workup

  1. custompurged 1-gallon bottle
  2. addition37.5 ml of the MoCl5 solution was charged last
  3. additionadded
  4. washThe beaker contents were washed five times with 4,000 ml water
  5. washper wash
  6. addition3.1 grams of Ethyl 712 antioxidant (4,4'-bis[2,6-di-t-butylphenol]) was added
  7. washafter washing
  8. customdried at 77° C. for 8 hours
  9. customA solid, ring-opened dicyclopentadiene/1-hexene copolymer was recovered

Sources & evidence

ORD record
ord-21163147a4954a94bafc3b6f07304056
Source dataset
uspto-grants-1979_01
Patent number
US04136247

Reaction notes

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