반응 #710049
ord-d42af2836cdc4d4a91d217596954d8b4
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후처리
- 1workup.ADDITIONThe reaction mixture is poured into 150 ml of cold,
- 2workup.DISTILLATIONdistilled water and trimethylsilylcyclopentadiene
- 3추출is extracted into diethyl ether
- 4기타The extract is rotary evaporated
- 5기타to remove the ethereal solvent
- 6workup.DISTILLATIONdistilled
실험 절차
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).