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1.
Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2(3H)-carboxamide (1) and N-(2-methoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxamide (2),were synthesized from the initial compound benzo[d]isothiazol-3(2H)-one (BIT) and characterized by 1 H NMR,IR and elemental analysis,respectively.The single crystals of compounds 1 and 2 were obtained and determined by X-ray diffraction analysis.The preliminary results of biological activity experiment show that some of the title compounds exhibited a favorable antimicrobial activity. 相似文献
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An efficient method for the synthesis of novel pyrido[3',2':4',5']thieno[3',2':2,3]pyrido [4,5:d][1,3]thiazolo[3,2-a]pyrimidine-4-one derivatives (5) has been developed using a Pictet-Spengler reaction between 2-(3-aminothieno[2,3-b]pyridin-2-yl)thiazolo[3,2-a] pyrimidin-5-one (3), which could be obtained from the condensation of 7-(chloromethyl)-5H-thiazolo[3,2-a]pyrimidin-5-one (1) with 3-cyanopyridine-2-thione (2) via Thorpe-Ziegler isomerization, and aromatic aldehydes under NH2SO3H as catalysis in good yields. 相似文献
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Five new 2-(amino/aroxy)-5-methylpyrimido[5,4-c]quinolin-4(3H)-one derivatives have been designed and synthesized via an aza-Wittig reaction, and the structure elucidation was accomplished using extensive 1D ((1)H, (13)C) and 2D NMR spectroscopic studies (COSY, HSQC and HMBC experiments). 相似文献
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设计合成了两种新型的以2-苯基苯并噻唑为荧光团、N-(2-吡啶甲基)胺为识别基团的铁离子荧光分子探针2-(4-N-2-吡啶甲胺基)苯基-1,3-苯并噻唑(A1)和2-(4-N,N双2-吡啶甲胺基)苯基-1,3-苯并噻唑(A2),化合物结构用UV,IR,1HNMR和13CNMR进行了表征,并考察了探针的荧光特性.结果表明荧光分子探针A2在CH3 CH2OH/H-12O(1∶1,V/V)溶液中,能从常见的金属离子中以95%的荧光淬灭率选择性地识别铁离子,对Fe3+线性响应范围在0.15~1.3 μ mol/L之间,且检出限达10 nmol/L. 相似文献
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A novel benzisothiazolin-3-one derivative, 2-(benzo[d]isothiazol-3-yloxy)-N-(3-cyano-1-(4-fluorophenyl)-1H-pyrazol-5-yl) acetamide(8), was synthesized from the initial compound benzo[d]isothiazol-3(2H)-one(BIT) 1 and 4-fluoroaniline 3. The structure of the target compound 8 was determined by elemental analyses, IR and 1H NMR. The single crystals of intermediate compound 6 and the target compound 8 were obtained and determined by X-ray diffraction analysis. The preliminary biological activity was also evaluated and the results showed the target compound exhibited a good anti-microbial activity. 相似文献
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Leonelli F Garofalo B La Bella A Lasta E Ceccacci F Migneco LM Marini Bettolo R 《Magnetic resonance in chemistry : MRC》2007,45(5):420-423
6-endo- and 6-exo-Hydroxybicyclo[2.2.2]octan-2-one and 1-methyl-6-endo- and 6-exo-hydroxybicyclo[2.2.2]octan-2-one ethylene acetals and ethylene dithioacetals 1-4 have been characterized by 1D and 2D NMR methods. 相似文献
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取代苯甲醛与4-氨基-5-(3,4,5-三甲氧基苯基)-1,2,4-三唑-3-硫酮(2)缩合生成5-(3,4,5-三甲氧基苯基)-4-取代苯基亚胺基-1,2,4-三唑-3-硫酮(3),再烷基加成化为新型5,6-2H-1,2,4-三唑[3,4-b][1,3,4]噻二嗪衍生物4.化合物结构经1HNMR 13C NMR,IR以及元素分析确认.采用噻唑兰(MTT)比色法进行化合物抑制人体前列腺癌细胞(PC3)体外活性测试,结果表明所合成的化合物具有不同程度的抑制PC3活性,其中化合物4a在10μmol·L-1浓度下对PC3的抑制率为75.9%. 相似文献
8.
The one-pot reaction between 2-aminobenzo[d]isothiazol-3-one and alkyl propiolates in presence of triphenylphosphine leads to the corresponding alkyl 4-amino-5-oxobenzo[f][1,4]thiazepine-3-carboxylates. A plausible mechanism of the reaction is proposed and unambiguous evidence for the structures is obtained from a detailed magnetic resonance spectral analysis. 1D and 2D NMR spectra such as COSY, 1H-13C and 1H-15N HSQC and HMBC heteronuclear correlations and an INADEQUATE experiment are reported and discussed. 相似文献
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Ru Shu Sun Yang Wang Peng Xia 《中国化学快报》2008,19(7):791-794
The esterifications of 9-(hydroxyimino)-4-methyl-8,9-dihydrofuro[2,3-h]chromen-2-one (4) with acid chlorides afforded normal oxime-esters 3a-e in 35-78% yields in presence of excessive 4-dimethylaminopyridine as the acid scavenger, whereas the reactions gave unexpected 8-substituted products N-(8-chloro-4-methyl-2-oxo-2H-furo-[2,3-h]chromen-9-yl)amides (5a-c) and 4-methyl-2,9-dioxo-8,9-dihydro-2H-furo[2,3-h]chromen-8-ylcarboxyloates (6d-e) by using excessive acid chlorides. The structures of 10 new compounds were determined by 1H NMR, 13C NMR, MS and HRMS, and the possible mechanism for the formation of unexpected products 5a--c and 6d-e was also proposed. 相似文献
10.
The crystal structure of the title compound 1-(4-fluorophenyl) -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5(1H) -one(C23H21FN4O2S,Mr = 436.5) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854(3) ,b = 17.2678(4) ,c = 18.1828(5) ,β = 99.364(2) °,V = 4332.58(18) 3,Z = 4,Dc = 1.338,F(000) =1824,μ = 0.185 mm-1,MoKa radiation(λ = 0.71073) ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I > 2σ(I) . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5(1H) -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions. 相似文献
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Sobarzo-Sánchez E De la Fuente J Castedo L 《Magnetic resonance in chemistry : MRC》2005,43(12):1080-1083
The new oxoisoaporphines 7H-dibenzo[de,h]quinolin-7-one, 5-methoxy-7H-dibenzo[de,h]quinolin-7-one, 5-methoxy-6-hydroxy-7H-dibenzo[de,h]quinolin-7-one, 5-hydroxy-7H-dibenzo[de,h]quinolin-7-one and 5-methoxy-6H-dibenzo[de,h]quinolin-6-one were prepared either by oxidation of their 2,3-dihydro derivatives or by heating (2'-(3,4-dihydro-6,7-dimethoxyisoquinolin-1'-yl)phenyl)methylbenzoate with an acetic acid/sulfuric acid mixture at 100 degrees C. The structures were confirmed and 1H and 13C NMR spectra were completely assigned using two-dimensional NMR techniques. 相似文献
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The 1H,13C and 15N NMR spectra of the reduction product of 2-(3-oxo-3,4-dihydroquinoxalin-2-yl)benzene diazonium salt with sodium sulfite were measured and analysed. It is shown that the reaction product corresponds to 1-(indazol-3-yl)-1,2-dihydro-benzimidazol-2-on and not 6H-quinoxalino[1,2-c] [1,2,3]benzotriazin-12(13H)-one as published previously. The correctness of the structure was confirmed by an independent synthesis. The observed 15N chemical shifts were compared with the predicted ones using the ACD/NNMR 9.01 program. 相似文献
16.
芳基伯胺与芳基溴在Pd(dba)2/P(t-Bu)3催化下于80 ℃甲苯溶液中反应生成芳基仲胺, 芳基仲胺再与3-溴苯并[de]蒽-7-酮在Pd(OAc)2/P(t-Bu)3催化下于120 ℃邻二甲苯溶液中反应生成苯并[de]蒽-7-酮类叔芳胺有机电致发光材料; 3-二苯基氨基苯并[de]蒽-7-酮与丙二腈反应生成2-(3-二苯基氨基)苯并[de]蒽-7-基亚基丙二腈. 产物的结构经1H NMR, 13C NMR, 13C (DEPT), HRMS光谱所证实. 用UV-Vis, PL, DSC测定了化合物的发光性能. 相似文献
17.
The synthesis of previously unreported 1-amino-6,7-dihydro-7-(hydroxymethyl)-4-nitropyrrolo[1,2-f]pyrimidin-3-(5H)-one starting from 2-amino-6-methylpyrimidin-3-one is described. 相似文献
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1H, 13C and 15N NMR measurements (1D and 2D including 1H--15N gs-HMBC) have been carried out on 3-amino-1, 2,4-benzotriazine and a series of N-oxides and complete assignments established. N-Oxidation at any position resulted in large upfield shifts of the corresponding N-1 and N-2 resonances and downfield shifts for N-4 with the exception of the 3-amino-1,2,4-benzotriazine 1-oxide in which a small upfield shift of N-4 was observed. Density functional GIAO calculations of the 15N and 13C chemical shifts [B3LYP/6-31G(d)//B3LYP/6-311+G(2d,p)] gave good agreement with experimental values confirming the assignments. The combination of 13C and 15N NMR provides an unambiguous method for assigning the 1H and 13C resonances of N-oxides of 1,2,4-benzotriazines. 相似文献
20.
以氰乙酸乙酯(氰乙酸)为起始原料,经酯化、缩合、氯化,然后与2-氨基-4-甲基苯并[d]噻唑反应,合成了20个新化合物4.所有化合物结构经过IR,1H NMR,13C NMR和元素分析确证.初步生物活性测试表明:在500μg·mL-1浓度下,该类化合物4具有一定的抗黄瓜花叶病毒(CMV)及抗烟草花叶病毒(TMV)室内活体治疗活性,其中化合物4b,4o,4q对CMV具有较好的活体治疗活性(抑制率分别为45.81%,43.20%,43.09%),化合物4d,4f,4h,4l对TMV具有较好的活体治疗活性(抑制率分别为45.68%,45.19%,45.86%,44.32%),对照药宁南霉素的活体治疗活性分别为56.31%,54.63%. 相似文献