Reacción #92001

ord-a17d2cdcd2c949aab7f4b4f023a6eabf

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    ExtracciónThe organic compound was extracted into ethyl acetate (2×100 mL)
  2. 2
    Lavadothe combined organic layer was washed with brine solution
  3. 3
    Secadodried over anhydrous MgSO4
  4. 4
    FiltraciónFiltration and concentration
  5. 5
    Otrogave the crude residue which
  6. 6
    Otrowas purified

Procedimiento

To a mixture of 3,5-dichlorophenol (16.3 g, 100 mmol), imidazole (14.98 g, 220 mmol), and triisopropylchlorosilane (21.21 g, 110 mmol) was added DMF (200 mL) at room temperature. The resulting brown solution was stirred for 15 h and then it was diluted with water (500 mL). The organic compound was extracted into ethyl acetate (2×100 mL) and the combined organic layer was washed with brine solution and dried over anhydrous MgSO4. Filtration and concentration gave the crude residue which was purified using an ISCO (400 g) column chromatography to obtain 31.1 g (97%) of (3,5-dichlorophenoxy)-triisopropylsilane as a colorless oil. EI(+)-HRMS m/e calcd. for C15H24Cl2OSi (M)+ 318.0973, obsd. 318.0971.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09447035B2uspto-grants-2016_09