HCID 178479818, compound → HCID 178504323, compound

HRID 1294044Notes

Reaction equation

HRID 1294044 reaction equation
Cl[Ru:2](Cl)[C:3]1[CH2:10][CH2:9][CH:8]=[CH:7]CCC=1.[CH3:12][Si:13](C1([Na])C=CC=C1)([CH3:15])[CH3:14].[CH:22]1([Na])[CH:26]=[CH:25][CH:24]=[CH:23]1>O1CCCC1>[CH3:12][Si:13]([Ru:2]([CH:3]1[CH:10]=[CH:9][CH:8]=[CH:7]1)[CH:22]1[CH:26]=[CH:25][CH:24]=[CH:23]1)([CH3:15])[CH3:14]

Participants

5

Reactant 3

HCID 178479818HCID 178479818, compoundHCID 178504167HCID 178504167, compoundHCID 178507085HCID 178507085, compound

Product 1

HCID 178504323HCID 178504323, compoundYield 4.3%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent3×

Conditions

Temperature
-78 °C

Procedure

Further separately, 5 g of dichloro(1,5-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 tetrahydrofuran solution of trimethylsilyl cyclopentadienyl sodium and the above tetrahydrofuran solution of cyclopentadienyl sodium were added dropwise to the solution at the same time in a stream of nitrogen over 1 hour. The resulting solution was stirred at −78° C. for 3 hours and heated to room temperature under agitation over 12 hours. After the resulting 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 0.23 g of trimethylsilyl cyclopentadienyl(cyclopentadienyl)ruthenium (yield rate of 4.3%).

Workup

  1. temperatureheated to room temperature under agitation over 12 hours
  2. customto be purified
  3. concentrationconcentrated
  4. customit was separated
  5. custompurified by a neutral alumina column again

Sources & evidence

ORD record
ord-779a73db81df4639bfa20ebbfb795c78
Source dataset
uspto-grants-2007_07
Patent number
US07238822B2

Reaction notes

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