Reaktionsgleichung
[H-].[Na+].[CH2:3]=[C:4]([CH2:7][OH:8])[CH2:5][OH:6].[C:9]([Si:13]([CH3:16])([CH3:15])Cl)([CH3:12])([CH3:11])[CH3:10].[Cl-].[NH4+]>O1CCCC1>[Si:13]([O:6][CH2:5][C:4](=[CH2:3])[CH2:7][OH:8])([C:9]([CH3:12])([CH3:11])[CH3:10])([CH3:16])[CH3:15]Komponenten
Versuchsvorschrift
Under argon atmosphere, to a suspension of sodium hydride (490 mg, 60 wt. % oil dispersion) in tetrahydrofuran (10 ml) were sequentially added 2-methylene-1,3-propanediol (1 ml) and tert-butyldimethylchlorosilane (2.22 g) at 0° C., and then the mixture was stirred at room temperature for 1 hour. To this reaction mixture was added a saturated aqueous solution of ammonium chloride, and the mixture was extracted with ethyl acetate. This organic layer was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=3/1) to give the titled compound (1.62 g).
Aufarbeitung
- customat 0° C.
- extractionthe mixture was extracted with ethyl acetate
- washThis organic layer was washed with a saturated aqueous solution of sodium chloride
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=3/1)
Quellen und Nachweise
- ORD-Eintrag
- ord-744fd6db4a024650b5257babfba9884b
- Quelldatensatz
- uspto-grants-2014_09
- Patentnummer
- US08846746B2
Verknüpfte Notizen
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