一锅煮法合成5-甲基四氢叶酸钙

One-pot Synthesis of Calcium 5-Methyltetrahydrofolate

以叶酸为原料,采用一锅煮法合成5-甲基四氢叶酸,用活性炭吸附和半胱氨酸、乙醇和水混合液洗脱进行提纯分离,再与氯化钙反应制备较稳定的5-甲基四氢叶酸钙,最佳反应条件为n(叶酸):n(硼氢化钠)=1∶12,甲基化时间为2h,甲基化温度为30℃,活性炭吸附时间为3h,洗脱时间为5h.此条件下5-甲基四氢叶酸钙收率为82.4%,纯度为92.7%.用HPLC,元素分析,IR,UV,1 H NRM,MS等方法对目标产物结构进行了表征.

5-methyltetrahydrofolic acid was synthesized from folic acid by one-pot method.It was separated and purified by adsorption with activated carbon and elution in virtue of cysteine-ethanol-water mix,then reacted with calcium chloride to obtain a more stable compound of calcium 5-methyltetrahydrofolic acid.The optimal reaction conditions were as follows:the molar ratio of folic acid and borohydride was 1∶12,methylation reaction time was 2 h,methylation reaction temperature was 30℃,the adsorption time of activated carbon is 3 hand the elution time is 5 h.The yield of calcium 5-methyltetrahydrofolate is 82.4%,with the purity of 92.7%.Its structure was characterized by HPLC,elemental analysis,IR,UV,1 H NRM,MS.