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目的为马来酸曲美布汀的重要中间体2-二甲氨基-2-苯基-1-丁醇的合成奠定基础。方法苯乙腈与溴乙烷进行烃化反应得2-苯基-1-丁腈,所得产物经水解得2-苯基-1-丁酸,然后通过硼氢化钠-碘体系还原得2-苯基-1-丁醇;苯乙腈与N-溴代丁二酰亚胺进行卤代反应得溴代苯乙腈,所得产物与二甲胺进行烃化反应得2-二甲氨基苯乙腈,然后与溴乙烷进行烃化反应得2-二甲氨基-2-苯基丁腈。结果合成了2-苯基-1-丁醇和2-二甲氨基-2-苯基丁腈,总收率为分别为51%和59.4%。目标产物的结构经核磁共振氢谱、质谱确证。结论本合成方法原料易得,操作简单,收率较高,适合于工业化生产。
The purpose of trimebutine maleate important intermediates 2-dimethylamino-2-phenyl-1-butanol synthesis basis. Methods Benzeneacetonitrile was reacted with bromoethane to obtain 2-phenyl-1-butyronitrile. The obtained product was hydrolyzed to give 2-phenyl-1-butyric acid and then reduced by sodium borohydride-iodine system to obtain 2-benzene 1-butanol; benzene acetonitrile and N-bromosuccinimide halogenated reaction of brominated phenylacetonitrile, the resulting product and dimethylamine alkylation reaction 2-dimethylaminobenzene acetonitrile, and then with Bromoethane alkylation reaction 2-dimethylamino-2-phenyl butyronitrile. As a result, 2-phenyl-1-butanol and 2-dimethylamino-2-phenylbutyronitrile were synthesized in total yields of 51% and 59.4%, respectively. The structure of the target product was confirmed by 1H nuclear magnetic resonance and mass spectrometry. Conclusion The synthesis method is easy to get raw materials, simple operation, high yield, suitable for industrial production.