声化学法制备格利雅试剂氯化苄基镁的研究
Grignard reagents-benzylmagnesium synthesized using a sonochemistry method
-
摘要: 采用声化学法制备出格利雅试剂氯化苄基镁,研究在固定超声功率和频率(500W,25kHz,12个换能器)条件下,溶剂、温度、原料摩尔比、镁粉状态、搅拌对产率的影响,并在此基础上设计正交实验优化各因素。采用气相色谱对产品进行了定性、定量分析,研究表明用声化学法制备格利雅试剂氯化苄基镁的最佳工艺条件为:以新鲜镁粉、氯化苄为原料,THF、乙醚或THF和乙醚的混合液为溶剂,水浴温度约为20℃,不搅拌,产率为81%。Abstract: Grignard reagent benzylmagnesium chloride was synthesized using a sonochemistry method. The effects of solvent types, temperature, raw material mol ratio, magnesite powder states and stir situation on the yield of products under fixed ultrasonic power and frequency was studied. Based on the studies the orthogonal experiment was carried out to optimize the factors. Gas chromatogram was performed to analyze the products qualitatively and quantitatively, showing the optimum conditions: fresh magnesium powder and benzyl chloride as raw material, solvent being THF, ether or solution of THF and ether, water bath temperature 20℃ and unstirred, and the yield 81%.