共查询到19条相似文献,搜索用时 109 毫秒
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报道了一种噻吩并[3,2-d]嘧啶-4(3H)-酮的简便、高效合成新工艺。巯基乙酸乙酯和2-氯丙烯腈在乙醇钠作用下进行环合制得3-氨基噻吩-2-甲酸乙酯,然后在乙酸乙酯中与氯化氢气体成盐进行分离。3-氨基噻吩-2-甲酸乙酯的盐酸盐直接与过量的甲酰胺关环制得噻吩并[3,2-d]嘧啶-4(3H)-酮,两步总产率约80%。 相似文献
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报道了一条合成杂环4-氯噻吩并[3,2-d]嘧啶的新工艺。室温下2-氯丙烯腈缓慢滴加到巯基乙酸乙酯和乙醇钠的乙醇溶液中,经环合反应制得3-氨基噻吩-2-甲酸乙酯,其溶于乙酸乙酯后通入氯化氢成盐进行稳定和分离。3-氨基噻吩-2-甲酸乙酯的盐酸盐直接在过量的甲酰胺中,于140℃下第二次关环生成噻吩并[3,2-d]嘧啶-4(3H)-酮。噻吩并[3,2-d]嘧啶-4(3H)-酮在甲苯为溶剂,三乙胺为碱,100℃条件下与三氯氧磷进行氯代制备了4-氯噻吩并[3,2-d]嘧啶。本工艺与传统氯代方法进行比较后的优点是避免了使用过量有毒的三氯氧磷,后处理简单安全。 相似文献
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[目的]寻找一条合成4-甲基-5-咪唑甲酸乙酯的新工艺路线。[方法]以乙酰乙酸乙酯、磺酰氯与甲酰胺为原料,采用一锅法合成一种用途广泛的多功能单体4-甲基-5-咪唑甲酸乙酯。[结果]通过实验,确定了一条合成4-甲基-5-咪唑甲酸乙酯的新工艺:以二氧六环为溶剂,环化时反应温度为120℃,反应时间为4 h,n(乙酰乙酸乙酯)∶n(磺酰氯)∶n(甲酰胺)为1∶1∶2,在该条件下,4-甲基-5-咪唑甲酸乙酯的产率为70%。[结论]该方法路线简单,原料易得,适合工业化生产。 相似文献
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《化学与生物工程》2016,(6)
以自制2-氨基-4-甲基-5-(1 H-1,2,4-三唑-1-基)-噻吩-3-甲酸乙酯、三苯基膦、芳基异氰酸酯、伯醇为原料,合成了6种新型的2-烷氧基-3-芳基-5-甲基-6-(1 H-1,2,4-三唑-1-基)噻吩并[2,3-d]嘧啶-4(3 H)-酮衍生物,其结构经~1 HNMR、MS和元素分析表征,并用6种常见农作物病菌对目标化合物的抑菌活性进行了测试。结果表明,在用药浓度为5×10~(-5)g·L~(-1)时,目标化合物均表现出一定的抑菌活性,其中以2-甲氧基-3-对氯苯基-5-甲基-6-(1 H-1,2,4-三唑-1-基)噻吩并[2,3-d]嘧啶-4(3 H)-酮的活性最高,对小麦赤霉病菌的抑菌率达到75%。 相似文献
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以2-氯噻吩、多聚甲醛为原料,以离子液体[C2mim]Br、[C3mim]Br、[C4mim]Br、[C5mim]Br、[C6mim]Br、[C7mim]Br、[C8mim]Br、[C12mim]Br、[Bmim]PF6、[Bmim]BF4、[Bmim]C4F9SO3和[Bmim]Cl为催化剂进行氯甲基化反应,得到产物2-氯-3-氯甲基噻吩。研究表明,离子液体可以促进2-氯噻吩的氯甲基化反应,具有相转移催化剂的效果,并且以[C4mim]Br和[C8mim]Br的催化效果为佳。反应最佳条件为:离子液体[C8mim]Br摩尔分数为5%(相对于2-氯噻吩),温度40℃,反应时间8h,产物产率可达92.1%。 相似文献
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2-Amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carbonitrile and ethyl-2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate were synthesised by reaction of cyclohexanone and sulphur with malononitrile and ethyl cyanoacetate respectively. These 2-aminothiophene derivatives were diazotised and coupled with a variety of coupling components to give azo dyes. The spectral properties of these dyes are reported. The dyes had generally good colouration and fastness properties on polyester. 相似文献
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Synthesis and Reaction Behaviour of N-(3-Chlorobenzo[b]thiophene-2-carbonyl)-imino-dithiocarbonic Derivatives 3-Chlorobenzo[b]thiophene-2-carbonyl-chloride 1 was treated with potassium rhodanide to afford the appropriate acyl isothiocyanate 3 , which adds nucleophilic agents as amines and thioles in good yields. Addition of methanethiole and subsequent alkylation of the dithiocarbamate 7 gives S, S-dimethylimino-dithiocarbonate 8 . 3-Chlorobenzo[b]thiophene-2-carboxamide 2 reacts with carbon disulphide and phenyl isothiocyanate by chlorine substitution and cyclisation to benzo[b]thieno[2, 3-e]thiazines 9, 10 or 11 . The structure of the final products were determined by analytical and spectroscopical dates. 相似文献
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Satish M. Chavan Vasant M. Patil Pankaj B. Aware Poonam S. Patil 《Journal of Sulfur Chemistry》2016,37(4):426-437
Poly substituted 3-aminothiophenes were successfully synthesized in good yields by using a one-pot protocol via ketene S,S-acetal as an intermediate in basic medium (K2CO3/N,N-dimethylformamide) followed by Dieckmann condensation with ethyl bromoacetate. Further, chemistry of thiophenes was explored using active functional groups such as C3–NH2, C4–CN and C5–SCH3 on the thiophene nucleus.
Synthesis of ethyl 3-acetamido-4-cyano-5-(methylthio)thiophene-2-carboxylate derivatives and ethyl 3-amino-4-carbamoyl-5-(methylthio)thiophene-2-carboxylate derivatives. 相似文献
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S. Tumkevicius 《Advanced Synthesis \u0026amp; Catalysis》1994,336(2):160-162
The reaction of ethyl N-(6-ethoxycarbonyl-2-methyl-thiothieno[2,3-d]pyrimidin-5-yl)formimidate ( 1 ) with methyl-hydrazine, N,N′-dimethyl- and N,N′-diphenylhydrazines separately in refluxing ethanol resulted in hydrolysis of formimidate group to give ethyl 5-amino-2-methylthiothieno[2,3-d] pyrimidine-6-carboxylate ( 2 ). The reaction on 1 with methyl-hydrazine without solvent afforded ethyl 5-amino-2-(1-methyl-hydrazino)thieno[2,3-d]pyrimidine-6-carboxylate ( 3 ), which underwent hydrazone formation with p-nitrobenzaldehyde to give 4 . Treatment of 1 with N,N-dimethylhydrazine afforded a mixture of 3-dimethylamino-7-methylthiothieno[2,3-d:4,5-d']dipyrimidin-4(3H)-one ( 5 ) and 2 . Displacement of methylthio group in 5 with morpholine, piperidine and 4-methylpiperazine gave the corresponding 7-substituted derivatives 6a-c . The reaction of 1 with para-substituted phenylhydrazines resulted in the formation of 3-(p-substituted phenylamino)7-methylthiothieno[2,3-d:4,5-d']dipyrimidin-4 (3H)ones ( 7a-c ). 相似文献
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以2-萘酚、氰乙酸乙酯、4-氯苯甲醛为原料,以六氢吡啶有机碱为催化剂,无水乙醇为溶剂,通过Knoevenagl-Cope缩合得到2-氨基-3-乙氧羰基-4-(4-氯苯基)萘并吡喃(1),1再与三苯基膦、六氯乙烷及三乙胺反应得到膦亚胺中间体(2)。2与4-氯苯基异氰酸酯在二氯甲烷的溶液中采用aza-Wittig反应,得到碳二亚胺(3)。3与乙醇反应,经乙醇钠催化关环,合成了2-乙氧基萘并吡喃并[2,3-d]嘧啶-4(3H)-酮。实验考察了反应温度、反应时间、溶剂诸因素对膦亚胺收率的影响。结果表明:在反应温度5℃、反应时间6 h、乙腈为溶剂的优化条件下,产物收率为87.8%。产物结构经IR、1H NMR、MS进行了表征。 相似文献
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J. D. Warthen Jr. R. T. Cunningham A. B. Demilo S. Spencer 《Journal of chemical ecology》1994,20(3):569-578
Differences in attractiveness of four individualtrans isomers of ceralure (CRL) [ethyl 4- (and 5-) iodo-trans-2-methylcyclohexane-1-carboxylate] for male Mediterranean fruit fly,Ceratitis capitata (Wiedemann), were investigated. One of the isomers, CRL-B1 (ethylcis-5-iodo-trans-2-methylcyclohexane-1-carboxylate) was significantly superior to the three othertrans-CRL isomers, CRL, trimedlure (TML) [1,1-dimethylethyl 4- (and 5-) chloro-trans-2-methylcyclohexane-1-carboxylate], and TML-C (1,1-dimethylethyl-cis-4-chloro-trans-2-methylcyclohexane-1-carboxylate) on an equal weight basis. 相似文献
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Min Ju Cho Jangwon Seo Kai Luo Kyung Hwan Kim Dong Hoon Choi Paras N. Prasad 《Polymer》2012,53(18):3835-3841
Four alkyl-substituted thiophene-3-carboxylate containing donor–acceptor (D–A) copolymers were designed, synthesized, and characterized. Thiophene-3-carboxylate was used as a weak electron acceptor unit in the copolymers to provide a deeper highest occupied molecular orbital (HOMO) level for obtaining a higher open-circuit voltage in polymer solar cells (PSCs). The resulting bulk heterojunction PSCs, made of the copolymers and [6,6]-phenyl-C71-butyric acid methyl ester (PC71BM), exhibited different short circuit currents (JSCs) and open-circuit voltages (VOCs), depending on the length of alkyl side-chain in the thiophene-3-carboxylate unit. Among all fabricated photovoltaic (PV) devices, PC2:PC71BM (1:1 wt. ratio) showed the highest efficiency with the highest JSC of 10.5 mA/cm2. Although PC5:PC71BM (1:1) displayed the highest VOC of 0.93 V, the device efficiency was observed to be poor, which is due to poor nanophase segregation. This comparison shows that the side-chain of thiophene carboxylate in these copolymers plays a very important role in the device efficiency. 相似文献