Using 3-O-methyl-D-chiro-inosito as starting material,through acetalation and mesylation the intermediate 3,which was subjected to hydrolysis to afford 3-O-Methyl-4-[(methylsulfonyl)oxy]-D-chiro-inositol 4 was obtaine...Using 3-O-methyl-D-chiro-inosito as starting material,through acetalation and mesylation the intermediate 3,which was subjected to hydrolysis to afford 3-O-Methyl-4-[(methylsulfonyl)oxy]-D-chiro-inositol 4 was obtained.Subsequently,the key epoxide 5 was obtained in excellent yield via an epoxidation from the compound 4.Finally,the process of opening of epoxy ring by azole-bases resulted in the novel carbocyclic azole nucleoside compounds 6-10 in the presence of 1,8-diazabicycloundec-7-ene(DBU) as catalyst,which appeared strong regioselectivity.展开更多
建立了一种柱前衍生化高效液相色谱法(HPLC)测定荞麦中D-手性肌醇(D-CI)含量的方法,对衍生化试剂及方法的重复性、稳定性、精密性及加标回收率进行了考察。得到衍生化条件为:苯甲酰氯0.2 m L,吡啶0.6 m L,反应温度70℃,反应时间60 min;...建立了一种柱前衍生化高效液相色谱法(HPLC)测定荞麦中D-手性肌醇(D-CI)含量的方法,对衍生化试剂及方法的重复性、稳定性、精密性及加标回收率进行了考察。得到衍生化条件为:苯甲酰氯0.2 m L,吡啶0.6 m L,反应温度70℃,反应时间60 min;色谱条件为:C18柱(4.6 mm×250 mm,5μm),以乙腈和超纯水为流动相进行梯度洗脱,流速为1.0 m L/min,柱温30℃,UV检测波长230 nm。结果表明,荞麦中的D-CI获得了很好的分离,D-CI在0.004~0.04 mg/m L内线性相关性好,R^2为0.999,加标回收率为98.40%~100.67%,所建立的方法稳定、灵敏、重现性好,可用于测定荞麦中D-CI含量定量分析。展开更多
文摘Using 3-O-methyl-D-chiro-inosito as starting material,through acetalation and mesylation the intermediate 3,which was subjected to hydrolysis to afford 3-O-Methyl-4-[(methylsulfonyl)oxy]-D-chiro-inositol 4 was obtained.Subsequently,the key epoxide 5 was obtained in excellent yield via an epoxidation from the compound 4.Finally,the process of opening of epoxy ring by azole-bases resulted in the novel carbocyclic azole nucleoside compounds 6-10 in the presence of 1,8-diazabicycloundec-7-ene(DBU) as catalyst,which appeared strong regioselectivity.
文摘建立了一种柱前衍生化高效液相色谱法(HPLC)测定荞麦中D-手性肌醇(D-CI)含量的方法,对衍生化试剂及方法的重复性、稳定性、精密性及加标回收率进行了考察。得到衍生化条件为:苯甲酰氯0.2 m L,吡啶0.6 m L,反应温度70℃,反应时间60 min;色谱条件为:C18柱(4.6 mm×250 mm,5μm),以乙腈和超纯水为流动相进行梯度洗脱,流速为1.0 m L/min,柱温30℃,UV检测波长230 nm。结果表明,荞麦中的D-CI获得了很好的分离,D-CI在0.004~0.04 mg/m L内线性相关性好,R^2为0.999,加标回收率为98.40%~100.67%,所建立的方法稳定、灵敏、重现性好,可用于测定荞麦中D-CI含量定量分析。
