反応 #580640

ord-be5a5e9bd307417482280af77262364b

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The solution was concentrated
  2. 2
    workup.ADDITIONthe residue was treated with diethylether (100 mL)
  3. 3
    workup.STIRRINGThe mixture was stirred for 1 hour during which time the formation of a precipitate
  4. 4
    ろ過The mixture was then filtered
  5. 5
    濃縮the filtrate was concentrated
  6. 6
    workup.DISTILLATIONThe residue was distilled under reduced pressure

実験手順

To a cooled (0° C.) solution of allyltrichlorosilane (4.9 mL; 34 mmol) in CH2Cl2 (50 mL) was added 1,8-Diazabicyclo[5.4.0]undec-7-ene (13 mL; 84 mmol). A solution of pinacol (4.0 g; 34 mmol) in CH2Cl2 (50 mL) was then added slowly and the resultant solution was warmed to room temperature and stirred for 12 hours. The solution was concentrated and the residue was treated with diethylether (100 mL). The mixture was stirred for 1 hour during which time the formation of a precipitate was observed. The mixture was then filtered and the filtrate was concentrated. The residue was distilled under reduced pressure to give 5.2 g (72%) of 2-allyl-2-chloro-4,4,5,5-tetramethyl-[1,3,2]dioxasilolane as a clear, colorless liquid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07534905B2uspto-grants-2009_05