反応 #710049

ord-d42af2836cdc4d4a91d217596954d8b4

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONThe reaction mixture is poured into 150 ml of cold,
  2. 2
    workup.DISTILLATIONdistilled water and trimethylsilylcyclopentadiene
  3. 3
    抽出is extracted into diethyl ether
  4. 4
    その他The extract is rotary evaporated
  5. 5
    その他to remove the ethereal solvent
  6. 6
    workup.DISTILLATIONdistilled

実験手順

Trimethylsilylcyclopentadiene and bis(trimethylsilyl)cyclopentadiene are prepared by the procedures of Kraihanzel et al., J. Amer. Chem. Soc., 90, 4701 (1968) and I. M. Pribytkova et al., J. of Organometallic Chem., 30, C57-C60 (1971). Sodium cyclopentadienide (44 g, 0.50 mole) is added to 150 ml of tetrahydrofuran. Chlorotrimethylsilane (54 g, 0.5 mole) is added dropwise slowly to the reaction and the stirring is continued for 3 hours. The reaction mixture is poured into 150 ml of cold, distilled water and trimethylsilylcyclopentadiene is extracted into diethyl ether. The extract is rotary evaporated to remove the ethereal solvent and the residue is vacuum distilled to give trimethylsilylcyclopentadiene, b.p. 41° C.-43° C. (16 mm).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04772734uspto-grants-1988_09