反应 #1256751

ord-4713cfaf08d949ef970c4be7798a0db9

反应方程式

[Cl-].[NH4+]
ammonium chloride
[Mg]
Magnesium
II
iodine
CC(C)[SiH](Cl)C(C)C
diisopropylchlorosilane
CCOCCCBr
1-Bromo-3-ethoxypropane
CCOCCC[SiH](C(C)C)C(C)C
liquid
收率 107.4%
CCOCCC[SiH](C(C)C)C(C)C
(3-Ethoxypropyl)diisopropylsilane
收率 107.4%

溶剂

反应条件

温度
60°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取the resultant mixture was extracted with pentane
  2. 2
    洗涤by washing with water six times
  3. 3
    干燥drying over sodium sulfate anhydrate
  4. 4
    其他The solvent was removed under reduced pressure, whereby the Compound 61a

实验过程

1-Bromo-3-ethoxypropane (5.85 g, 35.0 mmol) was dissolved in THF (30 mL). Magnesium (900 mg, 37.0 mmol) and iodine (catalytic amount) were added thereto, and the resultant mixture was stirred at room temperature for 30 minutes and at 60° C. for 10 minutes. The resultant mixture was added dropwise to diisopropylchlorosilane (5.12 mL, 30.0 mmol) in THF (40 mL), followed by stirring at room temperature for 15 minutes and at 60° C. for 1.5 hours. Saturated aqueous ammonium chloride was added thereto, and 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 61a was obtained as an yellow liquid (6.52 g, 92%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07825103B2uspto-grants-2010_11