三种重要甘露糖衍生物的合成方法改进及微波辅助合成

Process improvement on three important mannose derivatives and their microwave assisted synthesis

对1,2,3,4,6-五-O-乙酰基-β-D-甘露糖、2,3,4,6-四-O-乙酰基-1-溴-α-D-甘露糖、3,4,6-三-O-乙酰基-1,2-O-烯丙氧基亚乙基-β-D-甘露糖这三种重要的甘露糖衍生物现有合成方法改进。同时首次通过微波辅助的方法合成了这三种产物,并在单因素实验的基础上,采用正交实验优化最佳合成工艺。结果表明微波辅助条件下,这三种物质的最佳合成工艺分别为:微波功率800W、反应时间20min、反应温度70℃、甘露糖与乙酸酐摩尔比1∶11;微波功率400W、反应时间50min、反应温度25℃、乙酸酐与溴化氢乙酸溶液体积比1∶3;微波功率500W、反应时间40min、反应温度30℃、2,6-二甲基吡啶与2,3,4,6-四-O-乙酰基-1-溴-α-D-甘露糖摩尔比1∶1。

The existing synthetic methods of 1,2,3,4,6-penta-O-aceytl-O-D-mannopyranose, 2,3,4,6-tetra- O - aceytl - 1 - bromide- a- D - mannopyranose, 3,4,6- tri - O - acetyl - 1,2- O - allyloxyethylidene- O - D - mannopyranose were modified in this paper. And the same time they were synthesized by the microwave assisted method firstly,and the best results were got by orthogonal experiment based on single factor investigation. Their optimum technology of synthesis were as follows ：800W,2Omin,70℃, molar ratio of mannose and acetic anhydride 1：11. 400W,50min,25℃, volume ratio of acetic anhydride and hydrogen bromide acetic acid solution 1：3. 500W, 40min, 30℃, molar ratio of 2,6-dimethylpyridine and 2,3,4,6-tetra-Q-aceytl- 1 - bromide-a-D-mannopyranose 1：1 .