^1HNMR技术在盐酸吡硫醇合成中的应用

APPLICATION OF 1HNMR IN SYNTHESIS OF PYRITINOL

应用１ＨＮＭＲ技术对盐酸吡硫醇合成的关键反应４，５－二（氯甲基）－３－羟基－２－甲基吡啶（２）的水解进行了研究。通过芳香环和甲基质子核磁信号的变化可方便地得知水解的过程，并计算出水解动力学参数。结果表明：在实验条件下，２能选择性地水解成所需的５－氯甲基－３－羟基－４－羟甲基－２－甲基吡啶（３），但不继续水解成吡多辛（ＶＢ６）。

HNMR technology was applied as a monitor in the hydrolysis of 4,5 bis (chloromethyl) 3 hydroxy 2 methylpyridine (2[STBZ]),the key step for synthesis of pyritinol.By observing the change of δ value and singal strength of aromatic and methyl proton in the course of hydrolysis,the kinetic constant of hydrolysis was easily calculated.The experimental results showed that 2 could be selectively hydrolyzed to the desired intermediate,5 chloromethyl 3 hydroxy 4 hydroxymethyl 2 methylpyridine (3).