Reacción #1504295

ord-3e234823c2164ce3a1c59ffc3ca28530

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroA 100 ml flask equipped
  2. 2
    Temperaturareflux condenser
  3. 3
    workup.STIRRINGThe suspension was stirred at 110° C. for two days
  4. 4
    FiltraciónThe solution was then filtered
  5. 5
    ExtracciónThe organic extract
  6. 6
    Otrochromatographed on silica using first cyclohexane
  7. 7
    Otroto collect the triallyl formyloxypropyl silane intermediate

Procedimiento

Triallyl (3-hydroxylpropyl) silane was prepared from triallyl-3-bromopropyl silane prepared in Example 7 via the formyloxypropyl intermediate. A 100 ml flask equipped with stir bar and reflux condenser was charged with 10.0 grams (36 millimoles) of triallyl 3-bromopropyl silane (prepared as described in Example 7), 4.90 grams (72 millimoles) sodium formate (commercially available from Aldrich Chemical Co. of Milwaukee, Wis.) and 0.60 grams of tetrabutyl ammonium bromide (commercially available from Aldrich Chemical Co.). The suspension was stirred at 110° C. for two days. The solution was then filtered and combined with equal volumes of deionized water and cyclohexane (commercially available as Omnisolve from E. Merck of Gibbstown, N.J.). The organic extract was flash chromatographed on silica using first cyclohexane, followed by 80/20 cyclohexane/acetone to collect the triallyl formyloxypropyl silane intermediate.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05876595uspto-grants-1999_03