2-甲基-3-硝基苯乙腈的新合成路线

目的改进2-甲基-3-硝基苯乙腈（合成罗匹尼罗所需的重要中间体）的合成路线。方法以2-甲基-3-硝基苯甲醛为原料,经还原、氯化和氰代等3步反应制取2-甲基-3-硝基-苯乙腈,新路线对文献报道的氯化和氰代进行了改进,用异丙醇/异丙醇铝代替了NaBH4,用二氯亚砜代替了三氯化磷或三溴化磷。结果 2-甲基-3-硝基苯乙腈单晶的结构经X-衍射得到确认,产率有了很大提高。结论采用新合成路线,原料易得,操作简便,成本低廉。

A New Synthesis Route of 2-Methyl-3-Nitrobenzene Acetonitrile

Objective To improve the synthetic procedure of 2-methyl- 3-nitrobenzene acetonitrile as the important intermediate of ropinirole synthesis. Methods 2- methyl- 3- nitrobenzaldehyde was the raw material and was prepared for 2- methyl- 3- nitrobenzyl cyanide by reduction,chloration and cyanation. Reduction and chloration reported by literature were improved in the new route by using isopropanol/ aluminium isopropoxide to replace sodium borohydride and thionyl chloride to replace phosphorus triehloride or phosphorus tribro- mide. Results The structure of the target compounds 2- methyl- 3- nitrobenzene acetonitrile monocrystalline was confirmed by X- ray, its yield was obviously improved. Conclusion The more convenient and efficient procedure is obtained by using the new synthesis route with easy operation and low cost.