2-{[4-(3-甲氧基丙氧基)-3-甲基吡啶-2-基]-甲硫基}1H-苯并咪唑的合成  

Synthesis of 2-{[4-(3-methoxypropoxy)-3-methylpyridine-2-yl]-methylthio}-1H- benzimidazole

作　　者：冯晓亮[1] 吾国强[1] 潘向军[1] FENG Xiao-liang;WU Guo-qiang;PAN Xiang-jun(Department of Chemical and Medical Engineering,West Branch of Zhejiang University of Technology,Quzhou 324000,China)

机构地区：[1]浙江工业大学浙西分校化学与制药工程系,浙江衢州324000

出　　处：《化学试剂》2006年第7期430-432,共3页Chemical Reagents

摘　　要：以2,3-二甲基-4-氯吡啶-N-氧化物为起始原料,经过取代、乙酰化、水解、氯化、缩合5步反应,制得了标题化合物,总收率42.48%,HPLC含量≥98.5%。通过IR、^(1)HNMR对产物进行了表征。4-(3-Methoxypropoxy)-2,3-dimethylpyridine N-oxide(1)was synthesized from 4-chloro-2,3-dimethylpyridine N-oxide,3-methoxypropanol and sodium in 88.8%yield.Heating 1 with acetic anhydride gave 2-acetoxymethyl-4-(3-methoxypropoxy)-3-methylpyridine(2)in 90%yield.Then 2 was hydrolyzed to 2-hydroxymethyl-4-(3-methoxypropoxy)-3-methylpyridine(3)in 75%yield.3 was halogenated with thionyl chloride to give 2-chloromethyl-4-(3-methoxypropoxy)-3-methylpyridine(4)in 76.2%yield.Finally,2-{[4-(3-methoxy propoxy)-3-methylpyridine-2-yl]-methylthio}-1H-benzimidazole(5)was synthesized by condensation of 4 and 2-mercapto-1H-benzimidazole in 93%yield.The purity of the product was up to 98.5%.The structure of the product was identified by IR and^(1)HNMR.

关 键 词：2 3-二甲基-4-氯吡啶-N-氧化物 2-{[4-(3-甲氧基丙氧基)-3-甲基吡啶-2-基]-甲硫基}1H-苯并咪唑 医药中间体 合成 

分 类 号：O626[理学—有机化学]