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对2,5-二甲基-3,4-二氢-4-氧代喹唑啉的合成进行了研究。以间甲基苯胺为原料经3步反应制得2-氨基-6-甲基苯甲酸,再环化生成2,5-二甲基-3,4-二氢-4-氧代喹唑啉。中间体及标题化合物结构经1 HNMR确证。 相似文献
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二甲基对溴碘代苯是带有两种不同卤素基团的芳香族有机合成中间体。2,6-二甲基苯胺在过碳酸钠作用下,于45~50℃与碘反应1 h,得到2,6-二甲基-4-碘苯胺,收率42.5%。2,6-二甲基-4-碘苯胺在-5~0℃下进行重氮化,进一步与溴化亚铜发生Sandm eyer反应,得到3,5-二甲基-4-溴碘苯,收率31.5%。2,6-二甲基苯胺室温下与六亚甲基四胺溴络合物反应30 m in,得到2,6-二甲基-4-溴苯胺,收率62.0%。2,6-二甲基-4-溴苯胺在-5~0℃进行重氮化,与K I反应,得到2,6-二甲基-4-溴碘苯,收率33.1%。通过熔点、红外光谱和核磁共振氢谱对中间体2,6-二甲基-4-碘苯胺、2,6-二甲基-4-溴苯胺以及最终产物3,5-二甲基-4-溴碘苯和2,6-二甲基-4-溴碘苯进行了表征。 相似文献
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6-溴甲基-3,4-二氢-2-甲基-4-氧代喹唑啉的合成 总被引:8,自引:0,他引:8
用对甲基苯胺与水合三氯乙醛、盐酸羟胺反应制得对甲基(N-肟基乙酰)苯胺,再与浓硫酸反应生成5-甲基靛红,后经碱性过氧化氢氧化,制得2-氨基-5-甲基苯甲酸。将2-氨基-5-甲基苯甲酸与硫代乙酰胺反应生成的3,4-二氢-2,6_二甲基4氧代喹唑啉,经N-溴代琥珀酰亚胺溴化得到标题化合物,其结构经IR,MS,^1HNMR和元素分析确证,5步反应总收率为23.1%。 相似文献
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为了制备2,6-二甲基-4-苯基-3,5-吡啶二甲酸,首先采取Hantzsch合成法,以0.10 mol苯甲醛、0.125 mol碳酸氢铵和0.25 mol乙酰乙酸乙酯为原料,在40 mL甲醇溶剂中回流0.5 h,合成了1,4-二氢-2,6-二甲基-4-苯基-3,5-吡啶二甲酸二乙酯,产率为45.9%;取0.01 mol 1,4-二氢-2,6-二甲基-4-苯基-3,5-吡啶二甲酸二乙酯在0.02mmol六水三氯化铁的醋酸水溶液中回流反应1 h进行芳构化合成了2,6-二甲基-4-苯基-3,5-吡啶二甲酸二乙酯,产率为50.2%;最后,2,6-二甲基-4-苯基-3,5-吡啶二甲酸二乙酯进行水解合成目标产物,产率为62.7%。 相似文献
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以3-氧代-4-甲酸甲酯四氢噻吩与氰化钠为原料,通过氰醇化、脱水、水解等反应合成了2,5-二氢噻吩-3,4-二羧酸酐(4),化合物4通过~1H NMR、~(13)C NMR、高分辨质谱(HRMS)等表征。研究了溶剂、反应温度以及不同配比的溶剂对合成2,5-二氢噻吩-3-4-二羧酸酐中间体的影响。制备3-氰基-4-甲酸甲酯-2,5-二氢噻吩(2)的较优条件为:POCl_3∶3-氰基-3-羟基-4-甲酸甲酯四氢噻吩(1)=2.5(物质的量比);制备2,5-二氢噻吩-3,4-二羧酸(3)的较优条件为:温度80℃,化合物2 1 g,乙酸2.9 mL,浓盐酸4.8 mL。对3-氰基-4-甲酸甲酯-2,5-二氢噻吩进行了~1H NMR、~(13) C NMR、HRMS表征。 相似文献
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Nathan C. Tice Sarah M. Peak Benjamin T. Cannon Ethan S. Laha Eli G. Estes Chad A. Snyder 《Journal of Sulfur Chemistry》2014,35(6):596-605
A general, convenient route toward N-substituted 5,6-dihydro-4H-thieno[3,4-c]pyrroles was accomplished by the reductive amination of 2,5-dimethylthiophene-3,4-dicarbaldehyde with various primary amines in a solution of sodium cyanoborohydride and methanol/acetic acid (80–88% yield). For the N-alkyl cases, the product isolated was the cyanoborohydride salt of the desired product, 1,3-dimethyl-5-alkyl-5,6-dihydro-4H-thieno[3,4-c]-5-pyrrolium cyanoborohydride. For the aryl case employing aniline, the desired free pyrrole, 1,3-dimethyl-5-phenyl-5,6-dihydro-4H-thieno[3,4-c]pyrrole, was isolated. X-ray crystallographic analysis of both the N-propyl and N-phenyl trials confirmed the salt and free amine nature of the products. 相似文献
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Tatsuji Chuman Keiko Mochizuki Masataka Mori Masahiro Kohno Kunio Kato Masao Noguchi 《Journal of chemical ecology》1985,11(4):417-434
A chemical study of the sex pheromone of the cigarette beetle was carried out. Seven components were isolated from active fractions of column chromatography of the female extract, and their structures were elucidated by spectroscopic evidence and confirmed by synthesis to be (4S,6S,7S)-4,6-di-methyl-7-hydroxynonan-3-one (serricornin) (I), 2,6-diethyl-3,5-dimethyl-3,4-dihydro-2H-pyran (anhydroserricornin) (II), 4,6-dimethylnonan-3,7-dione (III), 4,6-dimethylnonan-3,7-diol (IV), 4,6-dimethyl-7-hydroxy-4-nonen-3-one (V), (2S,3R)-2,3-dihydro-3,5-dimethyl-2-ethyl-6-(l-methyl-2-oxobutyl)-4H-pyran-4-one (serricorone) (VI) and (2S,3R)-2,3-dihydro-3,5-dimethyl-2-ethyl-6-(1-methyl-2-hydroxybutyl)-4H-pyran-4-one (serricorole) (VII).These structural features suggested that the occurrence of these components might be related to the polyketide biosynthesis. The behavioral bioassay and BAG experiments revealed the biological role of each component in the copulatory behavior of this insect. 相似文献
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K. Mochizuki M. Mori T. Chuman M. Kohno A. Ohnishi H. Watanabe K. Mori 《Journal of chemical ecology》1986,12(1):179-186
Reinvestigation of the pheromonal activity of anhydroserricornin, (2S,3S)-2,6-diethyl-3,5-dimethyl-3,4-dihydro-2H-pyran, showed that the magnitude of its activity was less than 1/103 of that of serricornin, 7-hydroxy-4,6-dimethyl-3-nonanone, the sex pheromone of the cigarette beetleLasioderma serricorne (F.). Neither a synergistic nor an inhibitory effect of anhydroserricornin addition on the action of serricornin was observed. 相似文献
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Mostafa M. Ghorab Marwa G. El-Gazzar Mansour S. Alsaid 《International journal of molecular sciences》2014,15(5):7539-7553
4-Aminoantipyrine was utilized as key intermediate for the synthesis of pyrazolone derivatives bearing biologically active moieties. The newly synthesized compounds were characterized by IR, 1H- and 13C-NMR spectral and microanalytical studies. The compounds were screened as anticancer agents against a human tumor breast cancer cell line MCF7, and the results showed that (Z)-4-((3-amino-5-imino-1-phenyl-1H-pyrazol-4(5H)-ylidene)methylamino)-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 5, 3-(4-bromophenyl) -1-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-4-oxo-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carbonitrile 13, 1-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1-Hpyrazol- 4-yl)-3-(4-iodophenyl)-4-oxo-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carbonitrile 14, 3,3′-(4,4′-sulfonylbis(4,1-phenylene))bis(1-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol- 4-yl)-4-oxo-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carbonitrile) 16, (Z)-1-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-2-hydrazono-4-oxo-3-phenyl-1,2,3,4-tetrahydropyrimidine-5-carbonitrile 17, (Z)-1-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-4-oxo-3-phenyl-2-(2-phenylhydrazono)-1,2,3,4-tetrahydro pyrimidine-5-carbonitrile 18, and (Z)-4-(3-amino-6-hydrazono-7-phenyl-6,7-dihydro pyrazolo[3,4-d]pyrimidin-5-yl)-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 19 were the most active compounds with IC50 values ranging from 30.68 to 60.72 μM compared with Doxorubicin as positive control with the IC50 value 71.8 μM. 相似文献
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以4-羟基-3-硝基苯甲酸为原料,经酯化、醚化、还原合环、硝化、水解等5步反应,合成了两个未见文献报导的化合物7-硝基-3-氧-3,4-二氢-2H-[1,4]苯并噁嗪-6-羧酸和8-硝基-3-氧-3,4-二氢-2H-[1,4]苯并嗪-6-羧酸,其结构经IR、LC/MS、1HNMR和元素分析确证。 相似文献
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用氮气冲洗、Sep PakC18固相萃取柱吸附和冷有机溶剂捕集提取烟熏腊鸡肉的挥发性成分,用色谱-质谱联用法测定结构,用气相色谱(FID检测器)法进行定量分析。结果表明,烟熏腊鸡肉的主要香气成分为11个酚及其衍生物,以及N 异丙基甲亚磺酰氨基 2 环己烯 2 酮、5 甲基 4 异丙烯基 4 己烯醛、4,6 二甲基 3 苯甲烯氨基 2 (1H)吡啶酮、3 (2,2 二甲基亚丙基)二环[3,3,1]壬烷 2,4 二酮、2,6 二叔丁基 4 羟基 4 甲基 2,5 环己二烯 1 酮、2,6 二叔丁基 4 亚甲基 2,5 环己二烯 1 酮、二苯胺、十八醛、6 甲氧基 1 吲哚 2 基 3,4 二氢 β 咔啉和2,5 二苯基 3 (2 糠酰)吡咯,其中酚及其衍生物主要提供烟熏香,烟熏腊鸡肉的挥发性成分与新鲜鸡肉的挥发性成分是不同的。 相似文献
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(2S)-6-氟-3,4-二氢-4-氧代-2H-1-苯并吡喃-2-羧酸是合成非达司他(一种口服醛糖还原酶抑制剂)关键中间体。该研究使用脂肪酶Novozym 435,对(±)-6-氟-3,4-二氢-4-氧代-2H-1-苯并吡喃-2-羧酸甲酯进行拆分,并对拆分反应条件进行了优化,确定了拆分的最适反应条件:乙腈-水溶液为溶剂,V(水)∶V(乙腈)=1∶4,m(酶)∶m(底物)=1∶10,在pH=7.0,温度40℃,时间为6 h条件下,得到的(2S)-6-氟-3,4-二氢-4-氧代-2H-1-苯并吡喃-2-羧酸的总收率为32.5%,对映体过量值为92.1%,为非达司他的制备提供了一条可行途径。 相似文献