Реакция #1256750

ord-5bd981af22ff45e48334337ac71934da

Уравнение реакции

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
Выход 103.1%
COCCC[SiH](C(C)C)C(C)C
Diisopropyl(3-methoxypropyl)silane
Выход 103.1%

Растворители

Условия реакции

Температура
55°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07825103B2uspto-grants-2010_11