3-氨基吡啶中间体合成工艺研究  

Study on the Systhesis of 3-Aminopyridine Intermediates

作　　者：傅胜辉 张先龙 吴超 李宁 温兰兰 吴李瑞 FU Sheng-hui;ZHANG Xian-long;WU Chao;LI Ning;WEN Lan-lan;WU Li-rui(Anhui Costar Biochemical Company Limited,Maanshan 243100,China)

机构地区：[1]安徽国星生物化学有限公司,安徽马鞍山243100

出　　处：《安徽化工》2023年第4期106-109,共4页Anhui Chemical Industry

摘　　要：以3-甲基吡啶为原料,采用钒、磷摩尔比为1∶1的VPO/SiO_(2)催化剂,反应温度300℃,3-甲基吡啶∶NH_(3)∶空气∶水蒸汽摩尔比为1∶7∶20∶6的条件下合成3-氰基吡啶,精馏得到3-氰基吡啶含量为98%,收率为97%;负压刮板薄膜蒸发器-0.06 MPa、175℃条件下回收精馏底料中的3-氰基吡啶;3-氰基吡啶、30%盐酸、四丁基溴化铵摩尔比为1∶4∶0.05,反应温度80℃,反应时间8 h,可制得含量为99%和产率为96%的烟酰胺。3-Cyanopyridine was synthesized at 300℃with 3-methylpyridine∶NH_(3)∶air∶water vapor molar ratio 1∶7∶20∶6 and VPO/SiO_(2) as catalyst with vanadium and phosphorus molar ratio 1∶1.The content of 3-cyanopyridine was 98%and the yield was 97%by distillation.The 3-cyanopyridine in the distillation residue was recovered by negative pressure scraper film evaporator under the condition of-0.06 MPa and 175℃.Nicotinamide was prepared at a molar ratio of 1∶4∶0.05 of 3-cyanopyridine,30%hydrochloric acid and tetrabutylammonium bromide at 80℃for 8 h.And the content of nicotinamide was 99%and the yield reached 96%.

关 键 词：3-氨基吡啶 3-甲基吡啶 3-氰基吡啶 烟酰胺 合成 

分 类 号：TQ253[化学工程—有机化工]