以2-氯吡啶(1)、2-甲氨基乙醇(2)和4-氟苯甲醛(4)为主要原料,经2步反应合成了4-{2-[N-甲基-N-(2-吡啶基)氨基乙氧基]}苯甲醛(5).第1步反应n(2)∶n(1)=4∶1,反应温度160℃,反应时间约6h,采用减压蒸馏进行后处理,2-[N-甲基-N-(2-吡啶基)氨基]乙醇(3)的收率在93％以上,过量2的回收率在97％以上,回收的2可以重复使用.第2步反应用氢氧化钠做碱性试剂,用甲苯和水分别做为两相的溶剂,在相转移催化剂CTAB作用下进行,经优化后5的收率可达90％以上.2步反应总收率达83％以上.%4-12-[N-Methyl-N-(2-pyridyl) ] aminoethoxy | benzaldehyde(5)was synthesized by a two-steps process with 2-chloropyr-idine(l) ,2-(methylamino) ethanol(2) ,and 4-fluorobenzaldehyde(4) as principal raw materials. In first step of the process, the mole ratio of 2 to 1 was 4:1 .reaction temperature 160℃ .reaction time about 6 h,and adopted vacuum distillation in work-up procedure. Under such conditions,the yield of 2-[n-methyl-n-(2-pyridyl)amino]ethanol(3) was more than 93% ,the rate of recovery of the excess 2 was more than 97% ,and recovered 2 could be cyclically used. The second step of process was carried out with sodium hydroxide as basic reagent,toluene and water as solvent of two phases respectively ,CTAB as phase-transfer catalyst,gave 5 in more than 90% yield under optimal conditions. The above two steps gave 5 in more than 83% overall yield.
展开▼
机译：前所未有的双核二硫代氨基甲酸镉加合物：双μ2-N-（2-羟基乙基基）-N-异丙基氨基甲酸氨基硫代氨基甲酸-κ3S：SS bis {N-（2-羟基乙基基）-N-异丙基氨基甲酰胺基硫基-κ2SS（3-{（（1E）-（E）-2-（吡啶-3-基甲基亚叉基）肼一-1-基叉基甲基基}吡啶-κN）镉二水合物
