تفاعل #1256750

ord-5bd981af22ff45e48334337ac71934da

معادلة التفاعل

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

المذيبات

ظروف التفاعل

درجة الحرارة
55°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07825103B2uspto-grants-2010_11