تفاعل #11993
ord-876474b7d56a4b3b88e8d5a4a4d44459
معادلة التفاعل
المتفاعلات
الكواشف
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المعالجة
- 1أخرىwhich had been flushed with inert gas
- 2أخرىwas provided with stopcock and magnetic stirrer bar
- 3ترشيحthe reaction mixture was filtered through a glass
- 4ترشيحfilter frit number 3 under inert gas
- 5غسيلThe filter cake was washed twice with 10 g of heptane
- 6أخرىsubsequently dried under reduced pressure
الإجراء التجريبي
3.4 g of rac-dimethylsilylbis(2-methylbenzo[e]indenyl)zirconium bis(3,5-di-tert-butylphenoxide) (IV) from example 1 were suspended in 35.8 g of toluene in a dry round-bottomed flask which had been flushed with inert gas and was provided with stopcock and magnetic stirrer bar. At room temperature, 7.5 g of a 10% strength by weight solution of acetyl chloride in toluene were quickly added to this suspension via a dropping funnel. The mixture was stirred at room temperature. After 4 hours, the reaction mixture was filtered through a glass filter frit number 3 under inert gas. The filter cake was washed twice with 10 g of heptane and subsequently dried under reduced pressure. This gave 1.7 g of the compound I as a yellowish powder. The 1H-NMR spectrum of the compound indicated the pure rac form.