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目的研究二去水卫矛醇的合成工艺。方法以植物提取的卫矛醇为起始原料,在0.16 mol·L-1溴酸溶液中进行溴代反应得到二溴卫矛醇(DBD),DBD和碳酸钾在叔丁醇中发生分子内消除反应得到二去水卫矛醇(DAG)粗品,经重结晶得到DAG纯品,并采用正交实验设计法对实验中所涉及的温度、溶剂用量和碱的用量等进行了优化。结果与结论本法原料易得,反应条件温和,后处理简便,适合放大生产,总收率为50%左右,产品纯度和有关物质均符合中华人民共和国药典规定。
Objective To study the synthesis of dianhydrogalactitol. Methods The didecitol (DBD) was obtained by the bromination of 0.16 mg · L -1 Bromic acid solution from dulcitol, which was extracted from plants. The DBD and potassium carbonate were intramolecularly formed in t-butanol After the reaction was completed, the crude DAG was obtained and the pure DAG was obtained by recrystallization. The orthogonal experimental design was used to optimize the temperature, amount of solvent and amount of base used in the experiment. Results and Conclusion The raw materials of this method are easy to obtain, the reaction conditions are mild, the post-treatment is simple and suitable for enlargement production, the total yield is about 50%, and the purity of the products and related substances are in accordance with the Pharmacopoeia of the People’s Republic of China.