Study On Synthesis Of2-Deoxy-D-ribose

As the basic raw materials and key intermediates of nucleoside drugs,2-deoxy-D-ribose is always focused on by researchers. The synthesis process of2-deoxy-D-ribose started from glucose and cyclohexanone is the most economically industrial route so far. However, this process is still reported to have week points such as low production yield, long reaction time and large amount of waste.Following important innovations are included in this paper and then synthetic methods are put forward.(1)Produced water is removed immediately by decompressing in the preparation step of disaccharide ketone, which is better for reaction yield and reduces the reaction time by half. Optimum process conditions of this step are:decompressing reaction pressure is200-500Pa(absolute pressure), holding temperature is20℃, sulfuric acid is0.35mol and cyclohexanone is420ml when glucose is1.00mol. Under above conditions, the reaction yield is3.6%higher than that of atmospheric reaction, which is analyzed in terms of reaction mechanism.(2)Continuous operation, which improves the reaction yield and makes the process more stable, is adopted to take the place of the traditional batch operation. When reaction temperature is95℃and residence time is8min which are the Optimum conditions of this step the reaction yield is1.6%higher than batch operation.(3)In the step of degradation, washing with methanol followed by crystallization lead to higher reaction yield simplified procedures. Optimum process conditions consist of amount of reaction solution100ml, methanol70ml, and aniline which is1.3times the amount of deoxyribose and added to the treat reaction solution to react about2h and the reaction solution is cooled to0～10℃and kept at that temperature for12h. The amide is obtained through treatment of filtering, washing and drying the above reaction solution and then reacted with benzaldehyde under the catalysis of benzoic acid to give refined2-deoxy-D-ribose with8%higher reaction yield.