Magnesium → HCID 178429897, compound

HRID 1739342Notes

Reaction equation

HRID 1739342 reaction equation
[Cl-].[Cl-].[CH-:3]1[CH:7]=[CH:6][CH:5]=[CH:4]1.[CH-:8]1[CH:12]=[CH:11][CH:10]=[CH:9]1.[Ti+2:13].[CH:14]1([N:20]=[CH:21][C:22]([CH3:30])=[CH:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1.[Mg]>C1COCC1>[CH:3]1([Ti:13]2([CH:8]3[CH:12]=[CH:11][CH:10]=[CH:9]3)[CH:23]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[C:22]([CH3:30])=[CH:21][N:20]2[CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:7]=[CH:6][CH:5]=[CH:4]1

Participants

5

Reactant 3

HCID 5462224MagnesiumHCID 54324058HCID 54324058, compoundHCID 124040768Titanocene dichioride

Product 1

HCID 178429897HCID 178429897, compoundYield 65.2%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a solution of 5.00 g (20.08 mmol) titanocene dichloride in 100 ml THF were added 4.57 g (20.08 mmol) 1-cyclohexyl-3-methyl-4-phenyl-1-aza-buta-1,3-diene and 0.83 g magnesium and the mixture was stirred at room temperature until the metal was fully reacted. The solvent was then removed to dryness in vacuo and the residue was extracted with 50 ml diethyl ether. 5.31 g 2,2-bis(cyclopentadienyl)-1-cyclohexyl-4-methyl-3-phenyl-1-aza-2-titana-cyclopent-4-ene were isolated from the diethyl ether extract as black crystals. (65% yield, characterised by 1H-NMR, 13C-NMR and elemental analysis).

Workup

  1. customwas fully reacted
  2. customThe solvent was then removed to dryness in vacuo
  3. extractionthe residue was extracted with 50 ml diethyl ether

Sources & evidence

ORD record
ord-e409c4f71097453bbaaa8cb986cbc496
Source dataset
uspto-grants-1999_10
Patent number
US05965678

Reaction notes

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