Nickel → 1271-28-9

HRID 1862195Notes

Reaction equation

HRID 1862195 reaction equation
[Ni:1].BrBr.[CH:4]1[CH2:8][CH:7]=[CH:6][CH:5]=1>C(COC)OC.C(NCC)C>[CH-:4]1[CH:8]=[CH:7][CH:6]=[CH:5]1.[CH-:4]1[CH:8]=[CH:7][CH:6]=[CH:5]1.[Ni+2:1]

Participants

6

Reactant 3

HCID 935NickelHCID 7612CyclopentadieneHCID 24408Bromine

Product 1

HCID 623901271-28-9

Reagents, catalysts & solvents 2

HCID 8021DiethylamineSolventHCID 80711,2-DimethoxyethaneSolvent

Procedure

29.4 g of nickel powder are suspended in 400 ml of dimethoxyethane and admixed while stirring with 27.3 ml of bromine. The mixture is stirred for 1 hour and the solvent is removed in an oil pump vacuum. The brown residue obtained is taken up in 400 ml of diethylamine while cooling in ice and admixed with 98 ml of freshly distilled cyclopentadiene. The suspension becomes green. After stirring for 12 hours at room temperature, residual solvent is removed in an oil pump vacuum and the product is isolated by Soxhlet extraction with 700 ml of petroleum ether.

Workup

  1. customthe solvent is removed in an oil pump vacuum
  2. customThe brown residue obtained
  3. temperaturewhile cooling in ice
  4. stirringAfter stirring for 12 hours at room temperature
  5. customresidual solvent is removed in an oil pump vacuum
  6. customthe product is isolated by Soxhlet extraction with 700 ml of petroleum ether

Sources & evidence

ORD record
ord-9bd348dab5104c99a6329c1b3e9d0191
Source dataset
uspto-grants-2003_03
Patent number
US06537943B1

Reaction notes

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