D-1-乙酰基-1,2,2,3-四甲基环戊烷的合成改进

Synthesis of D-1-acetyl-1,2,2,3-tetramethylcyclopentane

对合成D 1 乙酰基1,2,2,3 四甲基环戊烷的方法进行了改进。研究了投料比、反应温度、反应时间等因素对中间体和标题化合物收率的影响。结果表明,中间体龙脑酰基二酯的最佳合成条件为:乙氧基镁丙二酸酯和D 龙脑酰氯的物质的量配比为1∶1 4,反应时间为4 h,反应温度为在乙醚溶液中回流;水解、脱酸的最佳条件为:在冰乙酸和浓H2SO4 混酸作用下,140 ℃剧烈回流40 h。在所拟最佳条件下,总收率可达56%。

The technology of synthesizing D-1-acetyl-1,2,2,3-tetramethylcyclopentane is improved in this paper with investigations made on the effect of the ratio of D-camphyl chloride to ethoxymagnesium malonic ester, the esterifying temperature and time on the yields of D-camphyl diesters and the title compound. Results show that the optimal esterifying conditions are the ratio of 1∶1.4 and the reaction time of 4 h under reflux. Besides, the optimal hydrolysis and deacidifying conditions are the reaction time of 40 h at 140 ℃ in the presence of HAc and H 2SO 4. Under the optimal conditions, the total yield comes up to 56%.