Study On The Synthesis Of Phantolide

This thesis was mainly a detailed introduction of the process for preparing phantolide by three steps:first preparing p-cymene with liquid-phase catalytic dehydrogenation from industrial dipentene, then preparing 1,1,2,3,3,5-hexamethylindan(HMI)by using five-carbon-hydrocarbon containing active group and p-cymene as materials, at last preparing phantolide by acylation of HMI with chlori-acytyl.In the part of preparing p-cymene, the thesis did research on the preparing process of using industrial dipentene as the materials with liquid-phase catalytic dehydrogenation. For this part, the thesis mainly researced the choice of the catalyst, the effect to the yield of p-cymene by catalyst preparation craft and the reaction condition. We has determined the best catalyst preparation craft:dipping time was 4 hours, dipping temperature is 80℃, the content of Pd is 6%, the pH of dipping liquid is 7.5, the restoring temperature is 70℃, the restoring time is 1 hour.And we also has determined the best reaction condition:The reaction temperature is 170-180℃, the catalyst amount used is 0.3% for suitable, the reaction time is 3 hours for suitable. And we knew when each time carries on the new response, if supplemented the new 0.03% catalyst can maintain to the p-cymene yield invariablely 7 times.In the part of preparing HMI, the thesis did research on the preparing process of using Tertiary amyl alcohol,2-methyl-2-butene as the materials respectively. Then using GC-MS, the main outgrowths in each reaction systems were analyzed.In the part of Tertiary amyl alcohol producing HMI, through single-factor-experiments, the best reaction condition was found as:the keeping reaction time was about 1.5 hours; the reaction temperature was -10-0℃;the quantity of sulfuric acid was about 125g, the molar Ratio of p-cymene and Tertiary amyl alcohol is 1:2 and in such a condition the yield of reaction was 40.89%.In the part of using 2-methyl-2-butene as the material, through single-factor-experiments, the best condition was found:reaction time was 4 hours:reaction temperature was 0℃, the quantity of p-cymene was 21.998, the quantity of cyclo-hexane was 28.6g, the quantity of p-cymene is 40.2g and the yieldof reaction was 67.25%.Through mechanism analyzing on the process of producing HMI, it was known that because the sulfuric acid is more Spoile than the aluminum chloride. And also the yield to ben high when we used the 2-methyl-2-butene as materials. So it was suitable for producing HMI in industry production.In the part of producing Phantolide, through single-factor-Experiments, the highest yield of reaction condition was confirmed as:reaction time about 4 hours; reaction temperature about 20℃; the quantity of chlori-acytyl about 8.5g; the quantity of aluminum chloride 20g and the yield of reaction was as high as 88.92%.