Magnesium → HCID 178429898, compound

HRID 1739340Notes

Reaction equation

HRID 1739340 reaction equation
[CH:1]1([Ti:6]([Cl:9])(Cl)Cl)[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH:10]1([N:16]=[CH:17][C:18]([CH3:26])=[CH:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1.[Mg]>C1COCC1>[Cl:9][Ti:6]1([CH:1]2[CH:2]=[CH:3][CH:4]=[CH:5]2)[CH:19]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:18]([CH3:26])=[CH:17][N:16]1[CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1

Participants

5

Reactant 3

HCID 5462224MagnesiumHCID 54324058HCID 54324058, compoundHCID 178479828HCID 178479828, compound

Product 1

HCID 178429898HCID 178429898, compoundYield 51%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a solution of 5 g (22.79 mmol) cyclopentadienyltitanium(IV) chloride in 100 ml THF were added 5.18 g (22.79 mmol) 1-cyclohexyl-3-methyl-4-phenyl-1-aza-buta-1,3-diene and 0.55 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. 4.36 g 2-chloro-2-cyclopentadienyl-1-cyclohexyl-4-methyl-3-phenyl-1-aza-2-titana-cyclopent-4-ene were isolated from the diethyl ether extract as dark brown crystals. (51% 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-593ff38494954896b852f27bcf82b023
Source dataset
uspto-grants-1999_10
Patent number
US05965678

Reaction notes

Loading…