HCID 131731268, compound → HCID 131731267, compound

HRID 1192851Notes

Reaction equation

HRID 1192851 reaction equation
[C:1]([C:5]1[N-:6][C:7]([C:15]([CH3:19])([CH3:18])[CH2:16][CH3:17])=[C:8]([C:10]([CH3:14])([CH3:13])[CH2:11][CH3:12])[N:9]=1)([CH3:4])([CH3:3])[CH3:2].[K+].[Cl-].CC1[C-](C)C(C)=C(C)C=1C.[Ru+2:32]>C1COCC1>[C:1]([C:5]1[N-:9][C:8]([C:10]([CH3:13])([CH3:14])[CH2:11][CH3:12])=[C:7]([C:15]([CH3:19])([CH3:18])[CH2:16][CH3:17])[N:6]=1)([CH3:4])([CH3:3])[CH3:2].[Ru+3:32].[C:1]([C:5]1[N-:9][C:8]([C:10]([CH3:13])([CH3:14])[CH2:11][CH3:12])=[C:7]([C:15]([CH3:19])([CH3:18])[CH2:16][CH3:17])[N:6]=1)([CH3:4])([CH3:3])[CH3:2].[C:1]([C:5]1[N-:9][C:8]([C:10]([CH3:13])([CH3:14])[CH2:11][CH3:12])=[C:7]([C:15]([CH3:19])([CH3:18])[CH2:16][CH3:17])[N:6]=1)([CH3:4])([CH3:3])[CH3:2]

Participants

4

Reactant 2

HCID 131731268HCID 131731268, compoundHCID 131731269HCID 131731269, compound

Product 1

HCID 131731267HCID 131731267, compoundYield 34.3%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

1.1 g (37 mmoles) of potassium(2-tert-butyl-4,5-di(1,1-dimethylpropyl)imidazolate) dissolved in 25 ml of THF were added to 1 g (0.0037 moles) of ruthenium (pentamethylcyclopentadienide) chloride dissolved in 75 ml of dry THF and the resulting mixture stirred overnight at room temperature. The solvent was then removed by vacuum, 100 ml of dry hexane then added and the resulting mixture thoroughly stirred then filtered. The hexane was then removed by vacuum to yield 1.13 g of crude ruthenium (2-tert-butyl-di(1,1-dimethylpropyl)imidazolate). (pentamethylcyclopentadienide). Structure confirmed by GCMS, parent ion detected at 499 mu. The structure was also confirmed by X-ray structural analysis of a sample of crude material which was sublimed then recrystallized from hexane. This shows the imidazolate and cyclopentadienide anions to both be coordinated eta-5 to ruthenium, see FIG. 21.

Workup

  1. customThe solvent was then removed by vacuum, 100 ml of dry hexane
  2. additionthen added
  3. stirringthe resulting mixture thoroughly stirred
  4. filtrationthen filtered
  5. customThe hexane was then removed by vacuum

Sources & evidence

ORD record
ord-2326e7374dfc401cbe1156f8b5718e42
Source dataset
uspto-grants-2014_03
Patent number
US08680289B2

Reaction notes

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