Tetrahydrofuran → Chloropropyldimethylvinylsilane

The above-synthesized 3-chloropropylchlorodimethylsilane (1) (15.6 g, 91.2 mmol) was dissolved in 50 mL of THF, to which 1.6 M vinylmagnesium chloride (85.6 mL, 137 mmol) was slowly added at 0°, and the mixture was stirred for 2 hours. After the reaction, the organic layer was extracted with aqueous NH4Cl solution and ether, and the organic layer was washed with aqueous saturated NaCl solution. The washed organic solution was dried with anhydrous MgSO4, and then filtered through celite to remove MgSO4. After evaporating the solvent, the resulting residue was purified by column chromatography (n-Hex:EA=10:1, Rf=0.78) to give 14.2 g (96% yield) of pure 3-chloropropyldimethylvinylsilane (2).

1. additionwas slowly added at 0°
2. customAfter the reaction
3. extractionthe organic layer was extracted with aqueous NH4Cl solution and ether
4. washthe organic layer was washed with aqueous saturated NaCl solution
5. dry with materialThe washed organic solution was dried with anhydrous MgSO4
6. filtrationfiltered through celite
7. customto remove MgSO4
8. customAfter evaporating the solvent
9. customthe resulting residue was purified by column chromatography (n-Hex:EA=10:1, Rf=0.78)

ORD 기록

ord-3c60c145b3eb4100943d26a2597b63e4

출처 데이터셋

uspto-grants-2012_06

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08197903B2