ChemicalBook CAS DataBase List Bis(cyclopentadienyl)dimethyltitanium

Bis(cyclopentadienyl)dimethyltitanium synthesis

6synthesis methods

Product Name:Bis(cyclopentadienyl)dimethyltitanium
CAS Number:1271-66-5
Molecular formula:C12H16Ti
Molecular Weight:208.12

Bis(cyclopentadienyl)dimethyltitanium is prepared by a solution of Methyllithium (2.1 equiv) in Et2O is added dropwise to a suspension of Dichlorobis(cyclopentadienyl)titanium in Et2O (3-5 mL mmol-1) cooled in an ice bath. After 1 h the reaction mixture is quenched with ice water, the ether layer is separated, dried over MgSO4, filtered and evaporated. The resulting bright orange crystals of the reagent, obtained in 95% yield, are dissolved in THF or toluene and stored in the dark, in the refrigerator or freezer.

1271-19-8 Synthesis

1271-19-8
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$6.00/5g

676-58-4 Synthesis

676-58-4
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$15.00/25ml

1271-66-5
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$119.00/25g

Yield:1271-66-5 85%

Reaction Conditions:

in tetrahydrofuran at -10 - 0; for 1.33333 h;Schlenk technique;Inert atmosphere;

Steps:

Experimental procedure and spectroscopic characterization: Dimethyltitanocene(Petasis Reagent 1) Cp2Ti(CH3)21-2
A Schlenk flask was charged with titanocene dichloride (5.0 g, 20.1 mmol)(Aldrich Co)in 50 mL of distilled THF under argon atmosphere. To the red suspension, cooled to -100C, was added dropwise methyl magnesium chloride (3M solution in THF-Aldrich Co)(14.9 mL, 44.8 mmol, 2.23 equiv.). The mixture was stirred for 80 minutes while slowlywarming to 0 0C, affording an orange solution. After cooling to -10 0C, 40 ml of waterwas cautiously added. The organic phase was washed with water (2 x 25 ml) and brine (1x 25 ml) and dried over MgSO4. Removal of the solvent on a rotary evaporator affordedthe crude product as an orange solid (3.9 g, 95%). Recrystallization from 15 ml ofpentane at -30 0C afforded crystalline product (3.5 g, 85%).1H NMR (C6D6): δ 0.05 (s, 6H, CH3), 5.68 (s, 10H, Cp). 13C NMR: δ 45.9, 113.2.

References:

Kobeissi, Marwan;Yazbeck, Ogaritte;Chreim, Yamama [Tetrahedron Letters,2014,vol. 55,# 15,p. 2523 - 2526] Location in patent:supporting information

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1271-19-8 Synthesis

1271-19-8
313 suppliers
$6.00/5g