4-硝基-N-甲基-邻苯二甲酰亚胺合成新工艺

研究了以甲苯为溶剂 ,苯酐、甲胺、硝酸为原料两步法合成 4 -硝基 -N -甲基 -邻苯二甲酰亚胺的方法。讨论了反应温度、溶剂、原料配比和反应时间等对反应产率的影响。结果表明 ,当苯酐和甲胺的摩尔比为 1 / 1 30 ,回流反应 5h时 ,苯酐转化率达 95% ,N -甲基 -邻苯二甲酰亚胺收率为 94 %。N -甲基 -邻苯二甲酰亚胺硝化工艺为 :N -甲基 -邻苯二甲酰亚胺和混酸 (n(浓硫酸 ) /n(硝酸 ) =3/ 1 )的摩尔比为 1 / 1 1 ,混酸在 2 0～ 30℃、0 5h内加完 ,然后在 55～ 6 0℃反应 4h ,得到 4 -硝基 -N -甲基 -邻苯二甲酰亚胺。产物质量分数为 98% ,收率为 81 %。通过红外光谱对产品结构进行了表征

New Synthesis Method of 4-Nitro-N-Methylphthalimide

Synthesis of 4-nitro-N-methylphthalimide(4-nitro-NMP) started from ph thalic anhydride(PA) and aqueous methylamine (MA) toluene solution through an im portant intermediate N-methylphthalimide(NMP).When mole ratio n(PA)/ n(MA)=1/1. 3,reactive refluxing for 5 h,conversion of PA reached 98%.Yield of NMP rea ched 94%.The NMP obtained was nitrated to end product (4-nitro-NMP)by mixed sulfuric and nitric acid,where n(NMP)/n(mixed acid)=1/1.1,n(H 2SO 4)/n (HNO 3)=3/1.Mixed a cid was added at 20～30 ℃,followed by reaction at 55～60 ℃ for 4 h to obtai n a yield of 81% of 4-nitro-NMP.The end product was identified by means of IR.