HCID 178479817, compound → HCID 178504171, compound

HRID 1294043Notes

Reaction equation

HRID 1294043 reaction equation
Cl[Ru:2](Cl)[C:3]1[CH2:10][CH2:9][CH2:8][CH2:7]C=CC=1.[CH3:12][Si:13]([C:16]1([Na])[CH:20]=[CH:19][CH:18]=[CH:17]1)([CH3:15])[CH3:14]>O1CCCC1>[CH3:12][Si:13]([C:16]1([Ru:2][C:3]2([Si:13]([CH3:15])([CH3:14])[CH3:12])[CH:10]=[CH:9][CH:8]=[CH:7]2)[CH:20]=[CH:19][CH:18]=[CH:17]1)([CH3:15])[CH3:14]

Participants

4

Reactant 2

HCID 178479817HCID 178479817, compoundHCID 178504167HCID 178504167, compound

Product 1

HCID 178504171HCID 178504171, compoundYield 13%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Conditions

Temperature
-78 °C

Procedure

Separately, 5 g of dichloro(cyclooctadienyl)ruthenium was dissolved in 200 ml of well dried tetrahydrofuran in a 500 ml flask whose inside had been substituted by nitrogen. This solution was cooled to −78° C., and the above synthesized tetrahydrofuran solution of trimethylsilyl cyclopentadienyl sodium was added dropwise to the above solution in a stream of nitrogen over 1 hour. The resulting solution was stirred at −78° C. for 3 hours and returned to room temperature under agitation over 12 hours. After the solution was let pass through a neutral alumina column in an argon gas atmosphere to be purified and concentrated, it was separated and purified by a neutral alumina column again to obtain 0.9 g of bis(trimethylsilylcyclopentadienyl)ruthenium (yield rate of 13%).

Workup

  1. additionwas added dropwise to the above solution in a stream of nitrogen over 1 hour
  2. waitreturned to room temperature under agitation over 12 hours
  3. customto be purified
  4. concentrationconcentrated
  5. customit was separated
  6. custompurified by a neutral alumina column again

Sources & evidence

ORD record
ord-84f53e542c964ee0b25092f6674a7c12
Source dataset
uspto-grants-2007_07
Patent number
US07238822B2

Reaction notes

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