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4—(6—甲氧基—8—喹啉偶氮)—邻苯二酚的合成及分析应用 总被引:1,自引:0,他引:1
合成了 4 (6 甲氧基 8 喹啉偶氮 ) 邻苯二酚 (MQAPC)。产品通过了元素分析、红外光谱、薄层色谱、核磁共振鉴定。用光度法测定了MQPAC的酸离解常数 ,pKa1=- 8.2 0、pKa2 =- 2 .98、pKa3=- 0 .35、pKa4 =10 .4 6、pKa5=13.17。MQAPC在碱性溶液中 ,与Ni(Ⅱ )形成配合物 ,λmax=5 85nm ,Δλ =113nm。在 0 .2~ 1.8μg·ml- 1范围内服从比耳定律。测定了人发及血清中的微量Ni(Ⅱ ) ,结果满意 相似文献
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通过E-[4-[2-(4-羟基苯基)乙烯基]吡啶与1,n-二溴烷烃亲核取代反应合成了4,4‘-[1,n-亚烷基双[(E)-2-(4-氧基苯)乙烯基]]双吡啶[n=2(Ia),3(Ib),4(Ic),6(Id)]。用元素分析、红外、紫外和质子核磁共振谱鉴定了Ia-Id的结构。将Ia-Id的稀溶液用中压汞灯和低压汞灯交替照射,发现其分子内光环加成反应的存在,并且随着亚烷基碳链的延长,反应速度加快。研究还发现锌离子可以与吡啶环上氮原子发生螯合作用使分子内光环加成反应加快。本文化合物荧光很弱,在较高浓度下有较强分子间激基缔合物荧光。 相似文献
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吡唑类化合物的研究(Ⅵ):—吡唑[3,4—e]并—1,2,4—三嗪和吡唑[3,4—e]并—1,2,3,4—四嗪衍生物的合成 总被引:1,自引:0,他引:1
合成了14种1-苯基-3-氨基-5-氧代-4-取代腙吡唑及其关环产物吡唑[3,4-e]并-1,2,4-三嗪和吡唑[3,4-e]并-1,2,3,4-四嗪衍生物,经元素分析,IR^1H NMR和MS确定了其结构,并讨论了一些化合物的IR和1H NMR波谱性质。 相似文献
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<正> C18H18O6·H2O, Mr = 348. 34, cis-isomer: orthorhombic, Cmc21, a = 16. 421(3), 6 = 11.978(1), c=8. 624(1)(?), V = 1696. 2(?)3, Z = 4, Dc= 1.293 gcm-3, λ(MoKα) = 0. 71073(?), μ = 0. 911cm-1, F (000) = 763, R = 0. 043, Rw = 0. 042 for 769 unique observed reflections. trans-Isomer : orthorhombic, Cmc21, a = 16. 503(2), b = 12. 297(2), c=8. 557(3) (?). V = 1736(?)3, Z = 4, Dc= 1.271 gem-3, λ(MoKα) = 0. 71073(?), μ = 0. 892cm-1, F (000) = 736, R=0.048, Rw = 0. 046 for 551 unique observed reflections. The configurations of the two molecules appear as butterflies. There is a Cm symmetry in the molecule of each isomer. 相似文献
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1,4-二锂四苯基-1,3-丁二烯与溴甲烷反应生成顺,顺-和顺,反-2,3,4,5-甲苯基-2,4-己二烯,其分子结构和比例由MS-NMR及X射线单晶分析所确定,讨论了产物的生成途径。 相似文献
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用二氧化硫脲合成4—甲基—4‘—氨基二苯醚的研究 总被引:1,自引:0,他引:1
4甲基4′氨基二苯醚是合成农药、染(颜)料、医药的重要中间体.传统的制备方法是由4 甲基4′硝基化合物(简称硝基物)在盐酸存在下用二氯化锡还原得到[1] ,该方法工艺成熟、产品质量好,但产率低,污染严重.陈其亮等报道了由硝基物催化加氢的方法[2],但存在设备投资大,操作繁锁等缺点.二氧化硫脲(Thiourea dioxide ,简称TD)是一种非常优良的还原剂,已广泛应用于有机合成的许多方面[3,4],但应用于标题化合物的制备未见报道,本文对此进行了研究,收到较好效果.合成路线如下: 相似文献
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<正> C22H28N2O3S.HCl, Mr = 436.9, triclinic,P1;a=8.557(3),b= 10.299(2),c= 13.894(2)A;α= 99.25(1),β=86.64(2),γ= 107.68(2)°;V= 1151.2(3)A3,Z= 2, DC = 1.27g/cm3,R=0.064. The torsion angle C(14)-C(1)-N(2)-0(19) in the title compound is 137.5 being much larger than that (106°) in R30730. The dihedral angle between mean planes of the thiophene ring and piperidine ring is about 83 . 相似文献
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Treatment of 4-amino-3-(1-aryl-5-methyl-1,2,3-triazol-4-yl)-5-mercapto-1,2,4-triazoles/2-amino-5-(1-aryl-5-methyl-1,2,3-triazole-4-yl)-1,3,4-thiadiazoles with benzaldehyde,acetone and ω-bromoacetophenone was tested and compared.The title compounds Schiff bases,amides,imidazolo [2,1-b]-1,3,4-thiadiazoles and 7H-s-triazolo[3,4-b]-1,3,4-thiadiazines have been confirmed by elemental analyses,^1H NMR,IR and MS spectra.All the compounds have also been screened for their antibacterial activities against B.subtilis,S.aureus and E.coli. 相似文献
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对-二甲氨基苯甲醛和苯基氨基硫脲缩合反应生成1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲(DMB), 产物能从溶液中析出单一手性对映体晶体. 用单晶X射线衍射技术测定了它的绝对构型, 晶体属正交晶系, P212121空间群, a=0.7870(2) nm, b=1.1560(2) nm, c=1.6668(3) nm, V=1.5164(5) nm3, Z=4, Dc=1.307 g/cm3, F(000)=632, μ=0.213 mm-1, 2557个可观测点[I>2s(I)]精修的最终残差因子: R=0.0409, wR=0.1061, Flack参数为0.00(9), 能够确定绝对构型. 化合物的晶体结构和大宗粉末样品的固体圆二色谱表明化合物在结晶过程中发生单一对映体的手性堆积. 相似文献
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《Journal of Coordination Chemistry》2012,65(13):2203-2211
(E)-4-(4-Methoxyphenoxy)-4-oxobut-2-enoic acid and its Ce(IV), Th(IV), and UO2(II) complexes were synthesized and characterized by MS, elemental analysis, IR, UV, TG-DTA, and NMR. The complexes have composition [CeL2(OH)2 · 2H2O] · H2O, [ThL2(OH)2 · 2H2O] · H2O, and [UO2L2 · 2H2O] · H2O. Molar conductance data confirm that the three complexes are nonelectrolytes. The IR and NMR results show that the carboxylates coordinate to the metal ions bidentate, and the ester carboxylic groups do not take part in coordination. Luminescence spectra of the ligand and complexes in DMSO at room temperature were also studied showing strong luminescence of the metal ions. 相似文献
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1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲的合成及手性晶体结构 总被引:1,自引:0,他引:1
对二甲氨基苯甲醛和苯基氨基硫脲缩合反应生成对二甲氨基苯甲醛缩氨基苯硫脲{1-[4-(dimethylamino)ben- zylidene]-4-phenylthiosemicarbazide}, 并从溶液中析出手性晶体. 元素分析、红外光谱、紫外光谱、核磁谱、质谱和X射线衍射测定其组成和结构. 晶体属正交晶系, P212121空间群, a=0.77038(14) nm, b=1.1428(2) nm, c=1.6726(3) nm, V=1.4726(5) nm3, Z=4, Dc=1.346 g/cm3, F(000)=632, μ=0.219 mm-1, 可观测点精修最终偏离因子: R=0.0407, wR=0.1157. 化合物的晶体结构和固态圆二色谱表明化合物在结晶过程中发生单一对映体的手性堆积. 相似文献
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首次合成了5-(4-硝基苯偶氮)-8-(4-甲苯磺酰氨基)-喹啉,测量了其酸离解常数。在非离子型表面活性剂存在下,试剂与钴(Ⅱ)在pH9.0~11.2范围内形成配合物,ε_(645)=1.01×10~5L·mol~(-1)cm~(-1),在H_2o_2作用下,于λ_((?)m)/λ_((?)x)=420nm/345nm产生强荧光,建立了一个操作简便快速、灵敏度高、选择性好的荧光分析新方法,线性范围2~32ppb,检测极限0.1ngCo(Ⅱ)/ml,用以测量了维生素B_(12)及生物样品中的痕量钴(Ⅱ)。探讨了H_2O_2对荧光增敏的机理。 相似文献
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The two diarylheptanoids (E)-1-(4'-hydroxy-3'-methoxyphenyl)-7-(4"-hydroxyphenyl) hept-4-en-3-one 1 (Gingerenone C) and (±)-5-hydroxy-1-(4'-hydroxy-3'-methoxyphenyl)-7-(4"-hydroxyphenyl)-3-heptanone 2 were synthesized from vanillin 3 and 4-hydroxybenzaldehyde 9. 相似文献
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YING Hua-Zhou SUN Mao-Tang LIU Tao HU Yong-Zhou① 《结构化学》2008,27(10):1171-1174
The title compound 2-(2-chloro-4-nitrophenyl)-4-(4-chlorophenyl)-3a,4- diethoxy- 2,3,3a, 4-tetrahydrochromeno[3,4-d][1,2,3]diazaphosphole 2 (C29H30Cl2N3O7P, Mr = 633.44) was synthesized and its structure was characterized by IR, MS, ^1H NMR, ^13C NMR, ^31p NMR, elemental analysis and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1^-, a = 9.1549(3), b = 10.7168(4), c = 17.6272(6)A, α = 102.9363(12), β = 90.2713(9), γ = 117.4265(10)°, V= 1484.41(9)A^3, Z= 2,μ(MoKa) = 0.323, F(000) = 658, Z= 2, De= 1.417 g/cm^3, the final R = 0.0687 and wR = 0.2066 for 4943 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the diazaphospholine ring is almost planar and the two ethoxy groups bonded on the 3a- and 4-positions are in trans configurations. Its antiproliferative activity was also tested in vitro against four human tumor cell lines. 相似文献