合成1-(β,γ-环氧丙氧甲基)-7-异丙基-4-甲基反应影响因素探讨

STUDY ON FACTORS AFFECTING THE SYNTHESIS OF 1(,EPOXYPROPOXYMETHYL)7ISOPROPYL4METHYLAZULENE

研究了７异丙基４甲基１甲醇和环氧氯丙烷在碱性催化条件下反应合成１（β，γ环氧丙氧甲基）７异丙基４甲基这一新化合物的影响因素，结果表明影响反应和得率的主要因素为催化剂、碱浓度、反应温度及反应时间。在浓ＫＯＨＨ２Ｏ溶液、惰性有机溶剂、相转移催化剂、４０～８０℃水浴等反应条件下，反应可在２～３ｈ内完成，得率达６４％

A suitable method and satisfied conditions have been found to synthesize the new reactive 1(,epoxypropoxymethyl)7isopropyl4methylazulene ( 1 ). The results showed that reaction between 7isopropyl4methyl1azulenemethanol ( 2 ) and epichlorohydrin could undergo only under elevated temperature in a strong alkaline solution with a PTC catalyst such as NMe4Br. Major factors affecting the reaction are: catalyst,alkaline concentration, temperature and reaction time. The suitable conditions are: concentrated KOH solution, 30 to 80 , 0.2 h to 5 h ,and a PTC catalyst.Under the above conditions, compound 1 was obtained at yield up to 64%.