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【答案】应助回帖
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sltmac: 金币+15, 翻译EPI+1 2013-04-22 09:26:21
Dicyclopentadienyl-dimethyl titanium(I):
In a 500mL flask with stirrer, under N2 protection, 200mL anhydrous ether and 11.5g(46mmol) powder Dicyclopentadienyltitanium dichloride are charged into. At 10-15℃, it is stirred for another 1 hour. And then 100mL 1.0mol/L MeLi/ether solution is dosed avoiding strong light exposure (in dark conditions).
After dosage the mixture is stirred shortly at room temperature, and quenched with ice water. After phase separation, the organic phase is dried with Na2SO4, and concentrated under vacuum in lower temperature. The orange crystal product is obtained.
The crude product is purified by dissolving into ca.200mL pentane at room temperature. During slowly cooled to ca.-80℃, compound I is obtained as long needle.
The compound must be stored indark conditions (avoiding light exposure) at lower temperature. Yield: 95%.
C12H16Ti (MW 208.2) Calc.(Ber.) Found(Gef.) ---Element analysis
Found MW204. Acid decomposition: 133.5mg product can generate 28.7 (Calc. 28.2) mL methane。
The compound I is slight soluable in common organic solvents. |
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