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1.
利用实时红外对由光引发剂2,2′,5-三(2-氟苯基)-4-(3,4-二甲氧基苯基)-4′,5′-二苯基-1,1′-二咪唑(WJ-HABI)、增感剂4,4—二(N,N′—二甲基氨基)苯甲酮(EMK)及供氢体N-苯基甘氨酸(NPG)组成的复合引发体系进行光聚合动力学研究.探讨了复合引发体系的浓度、不同配比、紫外光的强度及... 相似文献
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氯化N-[5′-(3′-甲硫基-6′-甲基)-1′,2′,4′-三嗪基]吡啶?盐(Ⅱ)在吡啶中于室温通入硫化氢或与硫化氢饱和的硫氢化钠反应,均得到3-甲硫基-5-巯基-6-甲基-1,2,4-三嗪(Ⅲ);于较高温度与硫化氢反应,得3,5-二巯基-6-甲基-1,2,4-三嗪(Ⅳ).二者均可于氢氧化钠溶液中与碘甲烷反应,得到3,5-二甲硫基-6-甲基-1,2,4-三嗪(Ⅴ).Ⅱ在呲啶水溶液中与邻甲苯酚、闻甲苯酚、苯酚、间硝基苯酚、邻硝基苯酚或对硝基苯酚作用,得到相应的5-取代苯氧基化合物(Ⅶ_(a-f));与硫酚作用,得5-苯硫基化合物(Ⅷ);在吡啶中与无水乙醇作用,得5-乙氧基化合物(Ⅸ).化合物Ⅱ在吡啶水溶液中与Ⅲ作用,得S-[5′-(3′-甲硫基-6′-甲基)-1′,2′,4′-三嗪基]-3-甲硫基-5-巯基-6-甲基-1,2,4-三嗪(Ⅻ);与3-甲硫基-5-氧代-6-甲基-4,5-二氢-1,2,4-三嗪(Ⅰ)作用,得N~4_[5′-(3′-甲硫基-6′-甲基)-1′,2′,4′-三嗪基]-3-甲硫基-5-氧代-6-甲基-4,5-二氢-1,2,4-三嗪(ⅩⅧ);与3-甲硫基-5-氧代-4,5-二氢-1,2,4-三嗪(ⅪⅩ)作用,得N~4-[5′-(3′-甲硫基-6′-甲基)-1′2′4′-三嗪基]-3-甲硫基-5-氧代-4,5-二氢-1,2,4-三嗪(ⅩⅩ);与3-甲硫基-5-氧代-4,5-二氢-1,2,4-三嗪-6-羧酸乙酯(ⅩⅩⅢ)作用,得N~4_[5′-(3′-甲硫基-6′-甲基)-1′,2′,4′-三嗪基]-3-甲硫基-5-羰基-4,5-二氢-1,2,4-三嗪-6-羧酸乙酯(ⅩⅪⅤ);与喹唑酮-4(ⅩⅩⅦ)作用,得N~3_[5′-(3′-甲硫基-6′-甲基)-1′,2′,4′-三嗪基]-4-氧代-3,4-二氢喹唑啉(ⅩⅩⅧ).这些化合物的结构系通过其水解反应、胺解反应、红外吸收光谱、紫外吸收光谱或核磁共振谱等研究予以证明.3-甲硫基-5-对硝基苯氧基-6-甲基-1,2,4-三嗪(Ⅶ_f)与苯胺或对甲苯胺反应,得到3-甲硫基-5-取代苯胺基-6-甲基-1,2,4-三嗪对硝基苯酚复合物(X_(a,b).后者用碱处理,得3-甲硫基-5-取代苯胺基-6-甲基-1,2,4-三嗪(Ⅺ_(a,b)及对硝基苯酚. 相似文献
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以3,5-二取代异噁唑-4-甲酰肼为基本原料制备关键中间体1-(3-对甲氧基苯基-5-甲基异噁唑-4-基)-4-芳基氨基硫脲(3a~3c);3在不同条件下经关环反应制得含有3,5-二取代异噁唑的2-芳氨基噻二唑(4a~4c),2-芳氨基噁二唑(5a~5c)和3-[3′-(4"-甲氧基苯基)-5′-甲基-异噁唑4′-基)-4-芳基-1,2,4-三唑-5-硫酮(6a~6c);6与碘甲(乙)烷反应合成了4-芳基-5-[3′-(4″-甲氧基苯基)-5′-甲基异噁唑-4′-基]-3-甲(乙)硫基-1,2,4-三唑(7a~8c),其结构经1H NMR,IR,MS和元素分析表征,其中4,5,7和8未见文献报道. 相似文献
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经1-[5′-氨基-1′-(4″-氯苯基)-1′,2′,3′-三唑-4′-甲酰基]-4-(3′-溴苯基)-3-氨基硫脲在浓硫酸作用下制得2-(3′-溴苯胺基)5-[5′-氨基-1′-(4″-氯苯基)-1′,2′,3′-三唑-4′-基]-1,3,4-噻二唑化合物.该化合物的晶体结构经X射线衍射分析确定,化合物属三斜晶系,P1空间群,a=1.1784(2),b=1.4455(2),c=1.1353(1)nm;α=100.68(1),β=109.50(1),γ=79.89(1)°;V=1.7779nm~3;分子式C~(16)H_(11)BrClN_7S,M_r=448.75;D_c=1.673g/cm~3,Z=4,μ=58.16cm~(-1),最终偏离因子 R=0.084,R_w=0.086.分析化合物的键长,键角数据表明,该分子具有离域π键结构. 相似文献
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以香草醛为起始原料,与1-溴-3-氯丙烷经烷基化反应后,再与盐酸羟胺反应制得4-(3-氯丙氧基)-3-甲氧基苯腈(3);3经硝酸硝化、铁粉还原后,与N,N-二甲基甲酰胺二甲缩醛反应制得N-[5-(3-氯丙氧基)]-2-腈基-4-甲氧基苯基-N,N-二甲基甲酰胺(6);6与3-氯-4-氟苯胺合环后与芳香醚经取代反应合成了7个新型的4-氨基喹唑啉衍生物(9a~9g),其结构经1H NMR,13C NMR,IR和元素分析表征。初步生物活性测定结果表明:在用药量为10μmol·L-1时,N-(3-氯-4-氟苯基)-7-[3-(2-氯基苯氧基)丙氧基]-6-甲氧基喹唑啉-4-胺(9d)和5-氯-2-【3-{4-[(3-氯-4-氟苯基)胺]-6-甲氧基喹唑啉}-7-氧丙氧基】苯甲醛(9g)对人乳腺癌细胞Bcap-37的抑制率分别为61.4%和78.9%。 相似文献
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以2,3-丁二酮为原料,依次与苯甲醛和对苯二甲醛经缩合反应制得4-{4,5-二[(E)-苯乙烯]-1H-咪唑-2-基)苯甲醛}(2);以对二氯苄作为连接链,2与其经取代反应制得4-{1-[4-(氯甲基)苄基]-4,5-二[(E)-苯乙烯]-1H-咪唑-2-基}苯甲醛(3);3与单羟基四苯基卟啉(4)连接合成了4-{4,5-二[(E)-苯乙烯]-1H-咪唑-2-基}苯甲醛共价键连单羟基四苯基卟啉化合物(5),其中2,3和5为新化合物,其结构经1H NMR,MS和元素分析表征。用荧光光谱研究了5中基团3与基团4之间的能量转移过程。结果表明,当激发取代基团3时,能量能够从基团3转移至基团4上。 相似文献
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以对苯二甲醚为原料,经甲酰化和溴代反应合成2,5-二甲氧基-4-溴苯甲醛(2)。以对甲氧基苯酚为原料,经烷基化、氯甲基化和Michaelis-Arbuzov反应合成亚膦酸酯(5);2和5经Horner-Wittig-Emmons反应合成了2,5-双(4′-溴-2′,5′-二甲氧基苯基乙烯基)-1-甲氧基-4-(2′-乙基己基氧基)苯(6),总收率44.7%,其结构经1HNMR,13C NMR和元素分析表征。UV-Vis和荧光光谱(FL)研究表明,6的UV-Vis和FL的λmax分别位于410 nm和479 nm,497 nm,是一种绿光的MEH-PPV型单体。 相似文献
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以9-芴甲酸为起始原料经亲核取代反应和N-酰基化反应制得N-(2,2,2-三氟乙基)-9-(4-溴丁基)-9H-芴基-9-甲酰胺(4);4'-(三氟甲基)-[1,1'-联苯]-2-羧酸与N-叔丁氧羰基-4-氨基哌啶反应制得中间体N-(1-叔丁氧羰基哌啶-4-基)-4'-(三氟甲基)-[1,1'-联苯]-2-甲酰胺(7);7在4 mol·L-1HCl二噁烷溶液中脱除保护基制得N-(哌啶-4-基)-4'-(三氟甲基)-[1,1'-联苯]-2-甲酰胺盐酸盐(8);8与4在K2CO3作用下反应制得洛美他派(9);9与甲磺酸经成盐反应合成了甲磺酸洛美他派,总收率36.4%,其结构经1H NMR,IR和HR-ESIMS确证。 相似文献
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咪唑啉酮;schiff碱;串联aza-wittig反应;合成;生物活性 相似文献
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以1-磺丁基-3-甲基咪唑硫酸氢盐离子液体(b)为反应介质,7-氨基头孢烷酸(7-ACA,2)为原料,与4-甲基-5-甲酰基噻唑经缩合反应制得(6R,7R)-7-氨基-3-[2-(4-甲基-5-噻唑)乙烯基]-8-氧代-5-硫-1-氮杂双环[4.2.0]辛-2-烯-2-羧酸(7-ATCA,1),其结构经1H NMR,13C NMR和IR表征。考察了离子液体及其用量,原料摩尔比r[n(4-甲基-5-甲酰基噻唑)∶n(2)],反应温度和反应时间对1收率的影响。在最佳反应条件[b为反应介质,b用量为20 m L,r=1.3,于65℃反应5 h]下,1收率可达90%以上。 相似文献
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N. V. Makarova M. N. Zemtsova I. K. Moiseev 《Chemistry of Heterocyclic Compounds》2001,37(10):1266-1269
1-Adamantyl bromomethyl ketone and 1-adamantylmethyl chloromethyl ketone react with potassium thiocyanate in dimethylformamide to give the corresponding thiocyanatoketones which cyclize under the influence of HCl into 4-(1-adamantyl) and 4(-adamantylmethyl)chlorothiazole respectively. 4-(1-Adamantyl)-2-amino-5-bromothiazole and its N-derivative were synthesized by the reaction of 1-adamantyl dibromomethyl ketone with thioureas and N-substituted thiourea in acetonitrile. 相似文献
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Kiran S. Hon Hemantkumar N. Akolkar Bhausaheb K. Karale 《Journal of heterocyclic chemistry》2020,57(4):1692-1697
Novel 1-benzyl-3-(4-fluorophenyl)-1H-pyrazole-4-carbaldehydes 3a to 3e were synthesized via Vilsmeier-Haack reaction of the appropriate 1-benzyl-2-(1-(4-fluorophenyl)ethylidene)hydrazines, derived from 4-fluoroacetophenone 1 with substituted 2-benzylhydrazines 2a to 2e . The base catalyzed condensation of 1-benzyl-3-(4-fluorophenyl)-1H-pyrazole-4-carbaldehydes 3a to 3e with 1-(4-fluoro-2-hydroxyphenyl)ethanone 4 gave (E)-3-(1-benzyl-3-(4-fluorophenyl)-1H-pyrazol-4-yl)-1-(4-fluoro-2-hydroxyphenyl)prop-2-en-1-ones 5a to 5e . On cyclization with dimethyl sulfoxide (DMSO)/I2, compounds 5a to 5e gave 2-(1-benzyl-3-(4-fluorophenyl)-1H-pyrazol-4-yl)-7-fluoro-4H-chromen-4-ones 6a to 6e . Structures of all novel compounds were confirmed by infrared (IR), proton nuclear magnetic resonance (1H NMR), carbon nuclear magnetic resonance (13C NMR), and mass spectral data. All the synthesized compounds were screened for their antibacterial activities. 相似文献
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以芳甲酰肼和对硝基苯甲酰氯为主要原料, 合成出了10个酰氨基硫脲化合物5a~5j, 其中有6个(5d, 5f~5j)为新化合物. 在无需任何酸性催化剂条件下, 将制得的酰氨基硫脲在DMF中加热回流直接脱水关环合成出了9个2-芳基-5-(4-硝基苯甲酰氨基)-1,3,4-噻二唑化合物6a~6i, 其中7个(6b~6d, 6f~6i)为新化合物. 利用IR和1H NMR证明了化合物5存在两种异构体. 目标产物的结构通过IR, 1H NMR和元素分析进行了表征. 相似文献
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F. Firoozi K. Javidnia M. Kamali A. Fooladi A. Foroumadi A. Shafiee 《Journal of heterocyclic chemistry》1995,32(1):123-128
Starting from readily available ethyl-4-nitropyrrole-2-carboxylate ( 1 ), substituted 1-methyl-2-(1,3,4-thiadiazol-2-yl)-4-nitropyrroles and 1-methyl-2-(1,3,4-oxadiazol-2-yl)-4-nitropyrroles were prepared. The reaction of 1 with diazomethane gave ethyl 1-methyl-4-nitropyrrole-2-carboxylate ( 2 ). Reaction of compound 2 with hydrazine hydrate afforded the corresponding hydrazide 3 . The reaction of 3 with formic acid yielded 1-(1-methyl-4-nitropyrrole-2-carboxyl)-2-(formyl)hydrazine ( 7 ). Refluxing of the latter with phosphorus pentasulfide in xylene yielded compound 6 in 40% yield. Reaction of compound 7 with phosphorus pentoxide afforded compound 9 . Reaction of compound 3 with 1,1′-carboxyldiimidazole in the presence of triethylamine yielded 2-(1-methyl-4-nitro-2-pyrrolyl)-1,3,4-oxadiazoline-4(H)-5-one ( 11 ). Refluxing compound 3 with cyanogen bromide in methanol gave compound 12 . Compound 13 could be obtained through the reaction of compound 3 with carbon disulfide in basic medium. Alkylation of compound 13 afforded the correspanding alkylthio derivative 14 . Reaction of 1-methyl-4-nitropyrrole-2-carboxylic acid ( 15 ) with thiosemicarbazide and phosphorus oxychloride gave 2-amino-5-(1-methyl-4-nitro-2-pyrrolyl)-1,3,4-thiadiazole ( 16 ). Sandmeyer reaction of compound 16 yielded 2-chloro-5-(1-methyl-4-nitro-2-pyrrolyl)-1,3,4-thiadiazole ( 17 ). Refluxing of the latter with thiourea afforded 2-(1-methyl-4-nitro-2-pyrrolyl)-1,3,4-thiadiazoline-4(H)-5-thione ( 18 ). Alkylation of compound 18 gave the corresponding alkylthio derivative 19 . Oxidation of the latter with hydrogen peroxide in acetic acid yielded 2-(1-methyl-4-nitro-2-pyrrolyl)-5-methylsulfonyl-1,3,4-thiadiazole ( 20 ). 相似文献
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Donohue BA Michelotti EL Reader JC Reader V Stirling M Tice CM 《Journal of combinatorial chemistry》2002,4(1):23-32
A library of 422 1-(2-thiazolyl)-5-(trifluoromethyl)pyrazole-4-carboxamides was prepared in five steps using solution-phase chemistry. The first step in the synthesis was the reaction of ethyl 2-ethoxymethylene-3-oxo-4,4,4-trifluorobutanoate with thiosemicarbazide, which is reported in the literature to afford a 1:1 mixture of ethyl 1-thiocarbamoyl-5-(trifluoromethyl)pyrazole-4-carboxylate and ethyl 1-thiocarbamoyl-3-(trifluoromethyl)pyrazole-4-carboxylate. We reassigned the structure of the product to be a single compound, ethyl 5-hydroxy-1-thiocarbamoyl-5-(trifluoromethyl)-4,5-dihydro-1H-pyrazole-4-carboxylate. This common intermediate was diversified by reaction with 17 alpha-bromoketones affording, in two steps, 17 1-(2-thiazolyl)-5-(trifluoromethyl)pyrazole-4-carboxylic acids. Scavenger resins were used to facilitate formation and purification of up to 27 amides from each of these acids in the last step. In addition, the Curtius reaction was applied to 12 of the acids followed by quenching with alcohols to afford a 108-member carbamate library. Certain compounds in the two libraries were toxic to C. elegans. 相似文献