甘露寡糖中间体的微波辅助合成

对3，4，6-三-O-乙酰基-1，2-O-亚乙基-β-D-甘露糖、1，2-O-亚乙基-β-D-甘露糖、4，6-O-苯亚甲基-1，2-O-亚乙基-β-D-甘露糖这3种重要的甘露寡糖中间体合成方法进行改进。同时首次通过微波辅助的方法合成了这3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3种物质的最佳合成工艺分别为：微波功率600 W、反应时间3.5 h、反应温度35 ℃、硼氢化钠质量2.5 g；微波功率600 W、反应时间30 min、反应温度30 ℃、甲醇钠质量0.4 g；微波功率800 W、反应时间1.5 h、反应温度35 ℃、对甲基苯磺酸质量0.2 g。优化后的产率分别为80.3%、98.3%、91.9%。
The existing synthetic methods of 3, 4, 6-tri-O-acetyl-1, 2-O-ethylidene -β-D- mannopyranose, 1, 2-O-ethylidene -β-D- mannopyranose, 4, 6-O- benzylidene-1, 2-O-ethylidene -β-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 600 W, 3.5 h, 35 ℃, mass of sodium borohydride 2.5 g；600 W, 30 min, 30 ℃, mass of sodium methoxide 0.4 g；800 W, 1.5 h, 35 ℃, mass of p-methylbenzene sulfonic acid 0.2 g. Their optimized yield were 80.3%、98.3%、91.9%