反応 #1256750

反応方程式

diisopropylchlorosilane

magnesium

iodine

ammonium chloride

1-Bromo-3-methoxypropane

→

liquid

収率 103.1%

Diisopropyl(3-methoxypropyl)silane

収率 103.1%

溶媒

THF

THF

反応条件

後処理

1. 1
   workup.STIRRINGby stirring at room temperature for 1 hour
2. 2
   その他After termination of exothermic reaction
3. 3
   抽出The resultant mixture was extracted with pentane
4. 4
   洗浄by washing with water six times
5. 5
   乾燥drying over sodium sulfate anhydrate
6. 6
   その他The solvent was removed under reduced pressure, whereby the Compound 60a

実験手順

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%).

出典