N-甲基-2-吡咯腈的合成改进
Improved synthesis of N-methyl-2-pyrrolecarbonitrile
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摘要: 以N 甲基吡咯(NMP)为起始原料,先与Vilsmeier试剂反应,经碳酸钠水解、二氯乙烷萃取制得N 甲基 2 吡咯醛(NMPA),此法溶剂回收利用率高、安全、易于工业化生产并降低了生产及污水处理费用 再以NMPA与盐酸羟胺经肟化制得N 甲基 2 吡咯肟(NMPAO),最后在醋酐中脱水制得N 甲基 2 吡咯腈 (NMPC) 在由NMPAO脱水制NMPC的过程后,经氢氧化钠水溶液中和,降低了体系的色度,萃取易于进行,产品收率74. 7%Abstract: N-methyl-2-pyrrolealdehyde was synthesized by the reaction of N-methylpyrrole with Vilsmerier reagent and by hydrolysis in Na_2CO_3 solution subsequently. Owing to Na_2CO_3 and dichloroethane instead of CH_3COONa and ether, the reformative process has effective solvent recovery and high security. After then, N-methyl-2-pyrrolecarbonitrile(MPC) was synthesized by oximation and dehydration of N-methyl-2-pyrrolealdehyde in hydroxylamined hydrochloride and acetic anhydride respectively. By neutralization of rea...