Titanocene dichloride synthesis
- Product Name:Titanocene dichloride
- CAS Number:1271-19-8
- Molecular formula:C10H10Cl2Ti
- Molecular Weight:248.96
2 NaC5H5 + TiCl4 → (C5H5)2TiCl2 + 2 NaCl
The reaction is conducted in THF. Work-up entails extraction into chloroform/hydrogen chloride and recrystallization from toluene. In the original literature, the structure was poorly understood. Each of the two Cp rings are attached to Ti(IV) through all five carbon atoms. In organometallic chemical jargon, this bonding is referred to as η5 (see hapticity).
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1271-19-8
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Yield:1271-19-8 91.3%
Reaction Conditions:
with triethylamine in N,N-dimethyl-formamide at 65; for 2 h;Inert atmosphere;Cooling with ice;
Steps:
6 Example 6
The reaction apparatus was taken out from the oven, and the reaction apparatus was set up under heat. Under nitrogen cooling, nitrogen gas was cooled for 10 minutes. Under the protection of nitrogen, 18 mL of DMF was added to the reactor, then 37.94 g of titanium tetrachloride was added, and the mixture was stirred for 20 minutes. The pressure funnel continued to slowly add 150 mL of DMF to the reactor. A yellow precipitate formed upon the start of the addition. The precipitate was slowly dissolved as the solvent was added to obtain a yellow solution. Then, the ice bath was removed and slowly added to the same constant pressure funnel. Diethylamine, the color of the solution changed from yellow to dark green. After the addition was completed, 105.76 g of cyclopentadiene was continuously added, heated to 65 ° C, refluxed for 2 hours, the reaction was completed, cooled to room temperature, and the solvent was evaporated under reduced pressure. Then, adding ice water and stirring for 15 minutes, a red precipitate was precipitated, filtered under reduced pressure and washed with a small amount of ice water for 5 times to obtain a red precipitate which was a crude dichlorotitanium dichloride; the crude dichlorotitanocene was sufficiently dissolved with DMF, and decompressed. After suction filtration, the filtrate was spin-dried, and the obtained liquid was recovered as a solvent. The obtained solid was weighed with ice-water-dichloromethane-ethanol mixture (ice water, dichloromethane and ethanol in a ratio of 0.2:1.8:1 by volume). Crystal was filtered to give a red needle-like crystals, and dried in vacuo to obtain titanocene dichloride, the resulting solid weighed 45.46g, yield 91.3%.
References:
CN108440606,2018,A Location in patent:Paragraph 0016-0021
482321-42-6
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1271-19-8
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