连续加压炔化反应合成脱氢芳樟醇

Synthesis of Dehydrolinalool by Continuous Ethynylation Process under Pressure

研究了以液氨为溶剂 ,在反应温度 35～ 4 0℃ ,压力 2 0～ 2 5MPa的条件下 ,6 甲基 5 庚烯 2 酮连续加压乙炔化反应制备脱氢芳樟醇工艺 ,考察了反应时间、物料量比对反应的影响 ,并对反应机理作了初步探讨。实验表明 ,反应温度 35～ 4 0℃ ,压力 2 0～ 2 5MPa ,n (6 甲基 5 庚烯 2 酮 )∶n (催化剂 )∶n(乙炔 )∶n(液氨 ) =7∶1∶5 1∶15 3,反应时间为 2 1h ,脱氢芳樟醇收率为 92 %～ 94 % ,产品经减压精馏后 ,脱氢芳樟醇质量分数大于 98%

A continuous process of base catalyzed reaction of acetylene and 6 methyl 5 hepten 2 one in liquid ammonia under pressure to produce dehydrolinalool is described.Thus,1 mole of catalyst is used with 7 moles of methyl 5 hepten 2 one,51 moles of acetylene and 153 moles of ammonia to form 6.4-6.6 moles of dehydrolinalool with a yield of 92%-94% at 35-40 ℃ under pressure of 2.0-2.5 MPa.The product is distilled at reduced pressure and consists of over 98% dehydrolinalool.Mechanism of the ethynylation reaction is discussed.