The title compound N-tert-butyl-N(-(2,4-dichlorobenzoyl)-N-[1-(4-chlorophenyl)- 1,4-dihydro-6-methylpyridazine-4-oxo-3-carbonyl]hydrazine [(C23H_21N4O3Cl3)2·1.5H_2O, Mr = 1042.60] was prepared by the reaction of ...The title compound N-tert-butyl-N(-(2,4-dichlorobenzoyl)-N-[1-(4-chlorophenyl)- 1,4-dihydro-6-methylpyridazine-4-oxo-3-carbonyl]hydrazine [(C23H_21N4O3Cl3)2·1.5H_2O, Mr = 1042.60] was prepared by the reaction of 1-(4-chlorophenyl)-1,4-dihydro-4-oxo-6- methylpyridazine-3-carboxylic acid with chloroformate ethyl ester, then with N′-tert-butyl-N- (2,4-dichlorobenzoyl) hydrazine in the present of triethylamine. The crystal structure has been determined by X-ray diffraction. The crystal belongs to Monoclinic, space group P21/c, with unit cell constants a =11.4948(9), b=12.7495(10), c=35.854(3) ?, β =92.964(2)°, Z=4, V=5247.6(7) ?3, Dc = 1.320 Mg/m3, F(000) = 2156 , μ (MoKa)= 0.385, R = 0.0661, wR = 0.1875, for 9151 observed reflections( I >2σ(I)). The structure is a dimer linked by intermolecular hydrogen bond which can be observed between N(1)- H...O(6), N(5)- H...O(3). The distances are 2.068 and 2.027? respectively.展开更多
采用四种不同的氨基保护法合成了九个 N 叔丁基 N (取代)苯甲酰肼,其中,氯甲酸苄酯保护法和氯甲酸苯酯保护法首次被用于该类化合物的合成,氯甲酸苄酯保护法具有反应条件温和、收率高、后处理简单及污染小等优点,适宜大规模工业生产。但...采用四种不同的氨基保护法合成了九个 N 叔丁基 N (取代)苯甲酰肼,其中,氯甲酸苄酯保护法和氯甲酸苯酯保护法首次被用于该类化合物的合成,氯甲酸苄酯保护法具有反应条件温和、收率高、后处理简单及污染小等优点,适宜大规模工业生产。但是,该法的局限性是当苯环上有氯、溴或硝基等取代基时,不宜采用该法。此时,Boc保护法和氯甲酸苯酯保护法适宜作为该法的补充。展开更多
Four N′-tert-butyl-N-substituted chrysanthemoyl urea derivatives have been synthesized through "substructure link way": substituted chrysanthemoyl chlorides were directly reacted with tert-butyl urea at abo...Four N′-tert-butyl-N-substituted chrysanthemoyl urea derivatives have been synthesized through "substructure link way": substituted chrysanthemoyl chlorides were directly reacted with tert-butyl urea at about 40 ℃ in the presence of acetonitrile. The structures of the target compounds(2a～2d) were characte- rized by 1H NMR, IR and elemental analysis. The preliminary bioactivity tests showed that compound 2d was active against Cucumber, Chenopodium, Radish and Sorgham. The inhibitory percentage to the root was over 70% and it was also active against the growth of stalks. Compound 2b showed a considerable insecticidal activity.展开更多
文摘The title compound N-tert-butyl-N(-(2,4-dichlorobenzoyl)-N-[1-(4-chlorophenyl)- 1,4-dihydro-6-methylpyridazine-4-oxo-3-carbonyl]hydrazine [(C23H_21N4O3Cl3)2·1.5H_2O, Mr = 1042.60] was prepared by the reaction of 1-(4-chlorophenyl)-1,4-dihydro-4-oxo-6- methylpyridazine-3-carboxylic acid with chloroformate ethyl ester, then with N′-tert-butyl-N- (2,4-dichlorobenzoyl) hydrazine in the present of triethylamine. The crystal structure has been determined by X-ray diffraction. The crystal belongs to Monoclinic, space group P21/c, with unit cell constants a =11.4948(9), b=12.7495(10), c=35.854(3) ?, β =92.964(2)°, Z=4, V=5247.6(7) ?3, Dc = 1.320 Mg/m3, F(000) = 2156 , μ (MoKa)= 0.385, R = 0.0661, wR = 0.1875, for 9151 observed reflections( I >2σ(I)). The structure is a dimer linked by intermolecular hydrogen bond which can be observed between N(1)- H...O(6), N(5)- H...O(3). The distances are 2.068 and 2.027? respectively.
文摘采用四种不同的氨基保护法合成了九个 N 叔丁基 N (取代)苯甲酰肼,其中,氯甲酸苄酯保护法和氯甲酸苯酯保护法首次被用于该类化合物的合成,氯甲酸苄酯保护法具有反应条件温和、收率高、后处理简单及污染小等优点,适宜大规模工业生产。但是,该法的局限性是当苯环上有氯、溴或硝基等取代基时,不宜采用该法。此时,Boc保护法和氯甲酸苯酯保护法适宜作为该法的补充。
文摘Four N′-tert-butyl-N-substituted chrysanthemoyl urea derivatives have been synthesized through "substructure link way": substituted chrysanthemoyl chlorides were directly reacted with tert-butyl urea at about 40 ℃ in the presence of acetonitrile. The structures of the target compounds(2a～2d) were characte- rized by 1H NMR, IR and elemental analysis. The preliminary bioactivity tests showed that compound 2d was active against Cucumber, Chenopodium, Radish and Sorgham. The inhibitory percentage to the root was over 70% and it was also active against the growth of stalks. Compound 2b showed a considerable insecticidal activity.
