Synthesis method of vinyloxytrimethylsilane
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In a three-necked flask, 100 ml of dry DMF, 51.1 g of dry Et3N (0.5 mol) (dried twice over KOH, distilled and dried over CaH2) and 43.6 g of distilled trimethylsilyl chloride (0.4 mol) were added in sequence (via syringe), and 43.9 g of dry acetaldehyde (1 mol) (dried over Na2SO4) was slowly added to the mixture through a dropping funnel for 1.5 h. The mixture was stirred at room temperature for about 44 hours, and then 50 ml of xylene was added to the brown reaction slurry, which was then distilled by a microdistillation apparatus. The resulting reaction mixture was heated to a maximum of 135°C with a thermometer monitoring the bottom temperature. The distillate was then diluted with 100 ml of xylene and washed three times with 100 ml of water. The organic phase was washed three times with 50 ml of saturated NH4Cl solution and finally washed twice with 50 ml of saturated NaHCO3 solution. The mixture was dried over anhydrous sodium sulfate. The distilled solution is fractionated using a 20 cm Vigreux column to obtain the target product molecule vinyloxytrimethylsilane.