【摘要】 以1,10-二溴癸烷、乙酰乙酸乙酯为原料,通过相转移催化缩合、粗产物不经分离,直接水解合成了麝香酮关键中间体2,15-十六烷二酮,收率78.6%。然后以TiC l4与不同的叔胺为催化剂,对2,15-十六二酮进行分子内羟醛缩合关环反应,成功合成了脱氢麝香酮,并确定了顺反异构的比例,实验表明,以TiC l4-i-Pr2NEt为关环催化剂环合收率为79.5%,顺反异构比例为1∶3,有较好立体选择性。产品用IR、MS1、HNMR进行了表征。更多还原

【Abstract】 Using 1,10-dibromodecane and ethyl acetoacetate as raw materials,by phase-transfer catalytic condensation and hydrolysis of the product without separation,the key intermediate for synthesizing muscone,2,15-hexadecanedione,was obtained in 78.6% yield.Then TiCl₄ with different tertiary amines was applied as catalyst to the intramolecular ring closing aldol condensation of 2,15-hexadecanedion to give dehydrogenated muscone,and the ratio of E/Z isomers was determined.The result indicated that TiCl₄-i-Pr₂NEt can make the yield of ring closure reaction to 79.5% with good stereoselectivity（E（trans-）/Z（cis-） isomers=3）.The product was confirmed by MS,¹HNMR and IR.更多还原