【目的】寻找具有除草活性及抑菌活性的新型化合物。【方法】以2-(2-硝基苯基)乙腈为原料,经缩合、氧化、还原、环化、取代5步反应,合成了5-(4,6-二甲氧基嘧啶-2-基)-1-取代-3,5-二氢苯并[e][1,4]氧氮杂卓-2(1H)-酮类化合物,对合成的化...【目的】寻找具有除草活性及抑菌活性的新型化合物。【方法】以2-(2-硝基苯基)乙腈为原料,经缩合、氧化、还原、环化、取代5步反应,合成了5-(4,6-二甲氧基嘧啶-2-基)-1-取代-3,5-二氢苯并[e][1,4]氧氮杂卓-2(1H)-酮类化合物,对合成的化合物进行核磁共振谱(1 H NMR)、质谱(MS)及元素分析,并分别测定合成衍生物的除草活性及抑菌活性。【结果】经1 H NMR、MS及元素分析确认,成功合成了15个新型的5-(4,6-二甲氧基嘧啶-2-基)-1-取代-3,5-二氢苯并[e][1,4]氧氮杂卓-2(1H)-酮类化合物5和6a^6n。生物活性试验结果表明,在450g/hm2的剂量条件下,目标化合物5、6a、6b和6c对芥菜,6m和6n对芥菜、反枝苋及小藜显示出30%~40%的除草活性。在200mg/L的质量浓度下,目标物6c、6h和6m对黄瓜白粉病表现出30%以上的抑菌活性。【结论】本研究合成的化合物具有一定的除草和抑菌活性,其结构具有进一步改造研究的价值。展开更多
The complexes of zinc chloride and zinc nitrate with 2 amino 4,6 dimethyl pyrimidine (ADMP) were prepared through reflux in alcohol. The compositions of the complexes Zn(ADMP)2Cl2 (b) and Zn(ADMP)2(NO3)2·4H2O (c)...The complexes of zinc chloride and zinc nitrate with 2 amino 4,6 dimethyl pyrimidine (ADMP) were prepared through reflux in alcohol. The compositions of the complexes Zn(ADMP)2Cl2 (b) and Zn(ADMP)2(NO3)2·4H2O (c) were determined by chemical and elemental analyses. The complexes were characterized by IR, XPS, 1H NMR and TG DTG techniques. The constant volume combustion energies of ADMP and the complexes, ΔcE, were determined by a precise rotating bomb calorimeter at 298.15K. They were (-3664.53±1.18)kJ·mol-1, (-7130.94±3.69)kJ·mol-1, and (-7637.87±5.71)kJ·mol-1. Their standard enthalpies of combustion,, and standard enthalpies of formation, , were calculated. They were (-3666.39±1.18)kJ·mol-1, (-7129.70±3.69)kJ·mol-1, (-7632.91 ±5.71)kJ·mol-1 and (19.09±1.43)kJ·mol-1, (-411.96±4.03)kJ·mol-1, (-1153.28±6.02)kJ·mol-1.展开更多
The title compound 3 was synthesized from diethylguanidine nitrate（2） obtained from diethylamine, CaCN2 and HNO3. The mixture consisted of 0.5 mol 2, 0.55 mol acetonyl propionate, 3 g benzyltriethylammonium chloride...The title compound 3 was synthesized from diethylguanidine nitrate（2） obtained from diethylamine, CaCN2 and HNO3. The mixture consisted of 0.5 mol 2, 0.55 mol acetonyl propionate, 3 g benzyltriethylammonium chloride, and 44 g NaOH was refluxed for 4 hours to give 85 g 3, in yield 94.6%.展开更多
Synthesis steps of 4,5 diamino 6 hydroxy 2 mercaptopyrimidine were improved on cyclocondensation of ethyl cyanoacetate with thiourea,nitrosation and reduction to obtain the product in 89% yield with high purity on ind...Synthesis steps of 4,5 diamino 6 hydroxy 2 mercaptopyrimidine were improved on cyclocondensation of ethyl cyanoacetate with thiourea,nitrosation and reduction to obtain the product in 89% yield with high purity on industrial scale.展开更多
文摘【目的】寻找具有除草活性及抑菌活性的新型化合物。【方法】以2-(2-硝基苯基)乙腈为原料,经缩合、氧化、还原、环化、取代5步反应,合成了5-(4,6-二甲氧基嘧啶-2-基)-1-取代-3,5-二氢苯并[e][1,4]氧氮杂卓-2(1H)-酮类化合物,对合成的化合物进行核磁共振谱(1 H NMR)、质谱(MS)及元素分析,并分别测定合成衍生物的除草活性及抑菌活性。【结果】经1 H NMR、MS及元素分析确认,成功合成了15个新型的5-(4,6-二甲氧基嘧啶-2-基)-1-取代-3,5-二氢苯并[e][1,4]氧氮杂卓-2(1H)-酮类化合物5和6a^6n。生物活性试验结果表明,在450g/hm2的剂量条件下,目标化合物5、6a、6b和6c对芥菜,6m和6n对芥菜、反枝苋及小藜显示出30%~40%的除草活性。在200mg/L的质量浓度下,目标物6c、6h和6m对黄瓜白粉病表现出30%以上的抑菌活性。【结论】本研究合成的化合物具有一定的除草和抑菌活性,其结构具有进一步改造研究的价值。
文摘The complexes of zinc chloride and zinc nitrate with 2 amino 4,6 dimethyl pyrimidine (ADMP) were prepared through reflux in alcohol. The compositions of the complexes Zn(ADMP)2Cl2 (b) and Zn(ADMP)2(NO3)2·4H2O (c) were determined by chemical and elemental analyses. The complexes were characterized by IR, XPS, 1H NMR and TG DTG techniques. The constant volume combustion energies of ADMP and the complexes, ΔcE, were determined by a precise rotating bomb calorimeter at 298.15K. They were (-3664.53±1.18)kJ·mol-1, (-7130.94±3.69)kJ·mol-1, and (-7637.87±5.71)kJ·mol-1. Their standard enthalpies of combustion,, and standard enthalpies of formation, , were calculated. They were (-3666.39±1.18)kJ·mol-1, (-7129.70±3.69)kJ·mol-1, (-7632.91 ±5.71)kJ·mol-1 and (19.09±1.43)kJ·mol-1, (-411.96±4.03)kJ·mol-1, (-1153.28±6.02)kJ·mol-1.
文摘The title compound 3 was synthesized from diethylguanidine nitrate（2） obtained from diethylamine, CaCN2 and HNO3. The mixture consisted of 0.5 mol 2, 0.55 mol acetonyl propionate, 3 g benzyltriethylammonium chloride, and 44 g NaOH was refluxed for 4 hours to give 85 g 3, in yield 94.6%.
文摘Synthesis steps of 4,5 diamino 6 hydroxy 2 mercaptopyrimidine were improved on cyclocondensation of ethyl cyanoacetate with thiourea,nitrosation and reduction to obtain the product in 89% yield with high purity on industrial scale.
基金2013年国家级大学生创新创业训练计划项目(201313256001)湖北师范学院硕士研究生创新科研基金项目(1051320130216)+1 种基金National Undergraduate Training Programs for Innovation and Entrepreneurship(201313256001)Postgraduate Innovation Scientific Research Foundation of Hubei Normal University(1051320130216)
