تفاعل #11993

ord-876474b7d56a4b3b88e8d5a4a4d44459

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىwhich had been flushed with inert gas
  2. 2
    أخرىwas provided with stopcock and magnetic stirrer bar
  3. 3
    ترشيحthe reaction mixture was filtered through a glass
  4. 4
    ترشيحfilter frit number 3 under inert gas
  5. 5
    غسيلThe filter cake was washed twice with 10 g of heptane
  6. 6
    أخرىsubsequently 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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07098354B2uspto-grants-2006_08