Lithium Chloride → HCID 86665004, compound

HRID 1192850Notes

Reaction equation

HRID 1192850 reaction equation
[Cl-:1].[Cl-].[Cl-].[C:4]([C:8]1[N:9]([Ti+3:21])[C:10]([C:17]([CH3:20])([CH3:19])[CH3:18])=[C:11]([C:13]([CH3:16])([CH3:15])[CH3:14])[N:12]=1)([CH3:7])([CH3:6])[CH3:5].[CH3:22][O-:23].[Li+].[Cl-].[Li+]>C1(C)C=CC=CC=1>[CH3:22][O-:23].[CH3:22][O-:23].[Cl-:1].[C:4]([C:8]1[N-:12][C:11]([C:13]([CH3:16])([CH3:15])[CH3:14])=[C:10]([C:17]([CH3:20])([CH3:19])[CH3:18])[N:9]=1)([CH3:7])([CH3:6])[CH3:5].[Ti+4:21]

Participants

5

Reactant 3

HCID 433294Lithium ChlorideHCID 4177230Lithium methanolate2×HCID 178441621HCID 178441621, compound

Product 1

HCID 86665004HCID 86665004, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

To a Solution of 0.500 g (1.28 mmol) of 2,4,5-tri-tert-butyl-imidazolyltitanium trichloride in 7 ml of toluene was added to 0.235 g (6.2 mmol) of lithium methoxide at RT. The slurry was agitated at RT for 2 days followed by 16 hours at 50° C. During the treatment the color of the slurry changed from deep red to yellow. Mixture of lithium methoxide and lithium chloride was filtered off and solvent was distilled under vacuum at 50° C. Residue analysis by 1H and 13C NMR indicated presence of a mixture of 2,4,5-tri-tert-butyl-imidazolyltitanium dichloride methoxide (˜13 mol %) and 2,4,5-tri-tert-butylimidazolyltitanium chloride dimethoxide (˜87 mol %):

Workup

  1. waitfollowed by 16 hours at 50° C
  2. filtrationwas filtered off
  3. distillationsolvent was distilled under vacuum at 50° C
  4. additionpresence of a mixture of 2,4,5-tri-tert-butyl-imidazolyltitanium dichloride methoxide (˜13 mol %) and 2,4,5-tri-tert-butylimidazolyltitanium chloride dimethoxide (˜87 mol %)

Sources & evidence

ORD record
ord-53fa616364a64f408ca2e0b057406648
Source dataset
uspto-grants-2014_03
Patent number
US08680289B2

Reaction notes

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