摘要
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).
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
1999年第5期193-196,共4页
Chinese Journal of Pharmaceuticals
关键词
盐酸吡硫醇
维生素B6
合成
羟基
甲基吡啶
pyritinol hydrochloride,pyridoxine (VB 6), 4,5 bis (chloromethyl) 3 hydroxy 2 methylpyridine,5 chloromethyl 3 hydroxy 4 hydroxymethyl 2 methylpyridine, hydrolysis, 1HNMR