ChemicalBook CAS DataBase List Pentamethylcyclopentadienylhafnium trichloride

Pentamethylcyclopentadienylhafnium trichloride synthesis

6synthesis methods

Product Name:Pentamethylcyclopentadienylhafnium trichloride
CAS Number:75181-08-7
Molecular formula:C10H15Cl3Hf
Molecular Weight:420.08

4045-44-7 Synthesis

4045-44-7
233 suppliers
$11.00/1g

13499-05-3
202 suppliers
$15.90/2.5g

Pentamethylcyclopentadienylhafnium trichloride

75181-08-7
43 suppliers
$63.10/1g

Yield:-

Reaction Conditions:

Stage #1:1,2,3,4,5-pentamethylcyclopentadiene with n-butyllithium in hexane;toluene at 20; for 15 h;Schlenk technique;
Stage #2:hafnium tetrachloride in hexane;toluene at 20; for 48 h;

Steps:

Example 1
In a flame-dried 1,000 mL Schlenk flask, 21.0 g (0.147 g) of pentamethylcyclopentadiene [C5 (CH3) 5H] Mol) was dissolved in 300 mL of toluene and maintained at 0 ° C. To the flask maintained at 0 , n-butyllithium 57 mL (0.147 mol) of a solution (2.6 M concentration in hexane solvent) was slowly added dropwise to form a reaction solution. The above- The solution was slowly warmed to room temperature, and then the reaction solution was stirred at room temperature for 15 hours. 15 The internal temperature of the stirred flask was again cooled to 0 DEG C, and thereto was added ZrCl4 After 34.3 g (0.147 mol) was slowly added dropwise, the reaction solution was slowly warmed to room temperature. Then, the formed reaction solution And stirred at room temperature for 48 hours. To the reaction solution flask stirred for 48 hours, an n-butyllithium solution (hexane 187 mL (0.485 mmol) of isopropyl alcohol and 29.2 g (0.485 mmol) of isopropyl alcohol were added to the solution, Dissolved in 200 mL of hexane and reacted to prepare an in-situ LiO I After slowly adding Pr while maintaining the Pr at 0 , slowly cooling to room temperature Lt; / RTI & gt; The reaction solution heated to room temperature was stirred at room temperature for 15 hours to complete the reaction. After completion of the reaction, the solvent and volatile by-products were removed under reduced pressure, and n-hexane (C6H14) 500 mL. Thereafter, the n-hexane extract was applied to a cellite pad and a glass frit Lt; / RTI & gt; filtered through a frit. The filtrate obtained by the filtration was placed under reduced pressure to remove the solvent, To obtain a yellow gel-type solid compound represented by the following general formula (2): & lt; EMI ID =

References:

UP Chemical Co.,Ltd;Han, Won Suk KR2015/35855, 2015, A Location in patent:Paragraph 0085; 0086; 0087; 0088; 0089; 0090