Reacción #1256750

ord-5bd981af22ff45e48334337ac71934da

Ecuación de reacción

CC(C)[SiH](Cl)C(C)C
diisopropylchlorosilane
[Mg]
magnesium
II
iodine
[Cl-].[NH4+]
ammonium chloride
COCCCBr
1-Bromo-3-methoxypropane
COCCC[SiH](C(C)C)C(C)C
liquid
Rendimiento 103.1%
COCCC[SiH](C(C)C)C(C)C
Diisopropyl(3-methoxypropyl)silane
Rendimiento 103.1%

Disolventes

Condiciones de reacción

Temperatura
55°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.STIRRINGby stirring at room temperature for 1 hour
  2. 2
    OtroAfter termination of exothermic reaction
  3. 3
    ExtracciónThe resultant mixture was extracted with pentane
  4. 4
    Lavadoby washing with water six times
  5. 5
    Secadodrying over sodium sulfate anhydrate
  6. 6
    OtroThe solvent was removed under reduced pressure, whereby the Compound 60a

Procedimiento

1-Bromo-3-methoxypropane (9.18 g, 60.0 mmol) was dissolved in THF (55 mL), and magnesium (1.53 g, 62.9 mmol) and iodine (catalytic amount) were added thereto, followed by stirring at room temperature for 20 minutes and at 55° C. for 5 minutes. The resultant mixture was added dropwise to diisopropylchlorosilane (8.88 mL, 52.0 mmol) in THF (65 mL) for 5 minutes, followed by stirring at room temperature for 1 hour. After termination of exothermic reaction, the resultant mixture was further stirred at 50° C. for 1.5 hours, and saturated aqueous ammonium chloride was added thereto. The resultant mixture was extracted with pentane, followed by washing with water six times and drying over sodium sulfate anhydrate. The solvent was removed under reduced pressure, whereby the Compound 60a was obtained as an yellow liquid (10.1 g, 89%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07825103B2uspto-grants-2010_11