反応 #518587

ord-2f55e915321c46e9b056324fc88fced8

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度then cooled to 0° C.
  2. 2
    workup.STIRRINGThe resulting white slurry was stirred for 4 hours at room temperature
  3. 3
    温度then heated
  4. 4
    温度to reflux for 20 minutes
  5. 5
    ろ過After filtration and aqueous work-up
  6. 6
    その他the solvent was removed in vacuo
  7. 7
    その他to give a colorless liquid

実験手順

To a 500 mL Schlenk flask containing magnesium turnings (2.71 g, 111.5 mmol) in diethyl ether (250 mL) was added dropwise a solution of 1-bromo-3-phenylpropane (20.0 g, 100.5 mmol) over 4 hours. The resulting pale yellow solution was stirred for 10 hours at room temperature then cooled to 0° C. and treated with allyldichlorosilane (7.085 g, 50 mmol) via syringe. The resulting white slurry was stirred for 4 hours at room temperature then heated to reflux for 20 minutes. After filtration and aqueous work-up, the solvent was removed in vacuo to give a colorless liquid. Yield: 86%. FTIR (NaCl, cm−1): 3083, 3066, 3021, 2927, 2842, 2069, 1598, 1569, 1488, 1456, 1142, 1067, 1025, 987, 920, 891, 834, 745, 701. 1H NMR (CDCl3): 7.28, 7.17, 5.74, 4.89, 4.54, 3.74, 2.62, 1.67, 0.64.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06660230B2uspto-grants-2003_12