共查询到19条相似文献,搜索用时 593 毫秒
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1,4-二氢-3H-2,3-苯并噁嗪-3-甲酸乙酯经过硝化、还原和重氮化溴代得到了7-溴-1,4-二氢-3H-2,3-苯并噁嗪-3-甲酸乙酯(C)。以Pd(OAc)2/R(+)BINAP(2,2'-二苯膦-1,1’-联萘)为催化体系,C与苯胺、N-甲基苯胺、对氟苯胺、对乙氧基苯胺、环己胺、吗啡、四氢吡咯及六氢吡啶等8种有机胺类化合物(Amine1~8),在氮气保护下,以碳酸铯为碱于干燥的甲苯中100℃反应16~24h,生成了相应的8种新的7-胺基取代的1,4-二氢-3H-2,3-苯并噁嗪-3-甲酸乙酯类化合物(D1—8),反应收率分别为83%、85%、71%、90%、72%、63%、75%和83%。通过^1HNMR、质谱和元素分析对这些化合物的结构进行了表征。 相似文献
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6-氨基-7-氟-2H-1,4-苯并口恶嗪-3(4H)-酮(Ⅱ)是合成除草剂丙炔氟草胺的关键中间体,该文采用雷尼镍催化加氢还原7-氟-6-硝基-2H-1,4-苯并口恶嗪-3(4H)-酮(Ⅰ)高收率的制得了目标化合物Ⅱ,确定了最佳合成工艺条件:反应温度80℃,反应时间5 h,催化剂用量为原料质量的5%,氢气压力6 MPa,产品的收率95.2%,质量分数98.5%,溶剂和催化剂循环使用5次,对收率和产品质量分数无影响。产品结构经元素分析、红外光谱、核磁共振确证。 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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以6,7-二溴-2,3-二氢苯并[b][1,4]二噁烯为原料,在正丁基锂(n-BuLi)作用下,得到苯炔中间体,再与呋喃发生Diels-Alder反应,得到目标化合物2,3,6,9-四氢-6,9-环氧萘[2,3-b][1,4]二噁烯,通过~1HNMR和ESI-MS对其结构进行确证,并对反应条件进行研究。确定最佳反应条件为:n(6,7-二溴-2,3-二氢苯并[b][1,4]二噁烯)∶n(呋喃)=1∶4、正丁基锂用量为n(n-BuLi)∶n(6,7-二溴-2,3-二氢苯并[b][1,4]二噁烯)=1.2∶1、反应溶剂为甲苯、室温反应20 min,在此条件下,产物收率为76.5%。 相似文献
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以8a-甲氧基-4,4a,5,8-四氢-1,2-苯并口恶嗪-3-羧酸乙酯(1a)为起始原料,经NaOH醇溶液和酸处理,在4-pyrrolidinopyridine和碳化双(环己基亚胺)(DCC)的存在下与3-氨基-7,8-二甲氧基香豆素(2)进行了酰胺化反应,合成了天然产物Trichodermamides的类似物T-1,总收率为61.6%,T-1通过了1HNMR,13CNMR,IR和元素分析等光谱学的结构表征;同时水解反应研究发现,含苯并口恶嗪双环结构的化合物1a可水解脱去酯基,而口恶嗪双环8a位上连有两个O的缩酮类似结构可稳定地保留。 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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研究了甲磺酸帕珠沙星的合成路线及工艺。以左旋氧氟沙星的中间体(S)-9,10-二氟-3-甲基-2,3-二氢-7-氧代-7H-吡啶[1,2,3-de][1,4]苯并噁嗪-6-羧酸乙酯为起始原料,经亲核取代反应、酯水解并选择性脱羧、环合、水解、Hofmann降解、成盐,制得甲磺酸帕珠沙星,总收率49.4%。其化学结构经元素分析、^1H NMR、^13C NMR、MS得以确证。该合成路线及工艺适合工业化大生产。 相似文献
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以左氧氟沙星中间体(S)-9,10-二氟-3-甲基-7-氧代-2,3-二氢-7-H吡啶[1,2,3-de][1,4]苯并噁嗪-6-羧酸乙酯为起始原料,经与氰乙酸乙酯进行亲核取代反应、水解脱羧、环合、水解、Hoffman降解,与甲磺酸成盐得甲磺酸帕珠沙星,总收率为38%,产品纯度符合药用标准。 相似文献
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The reaction of 2,3-dichloronaphthazarin 1a with potassium 2-amino-benzenethiolate gives the ring-closure product 10,11-dithia-5H,16H-5, 16-diazadinaphtho[2,3a],[2,3c]-1,4-naphthoquinone 9 in 86.2% yield together with small amounts of 5-hydroxy-6-chloro-7-thia-12H-12-azanaphtho[2,3a]-1,4-naphthoquinone 8. Dye 9 is green in colour and absorbs infrared light at 727 nm. Oxidation of 9 by hydrogen peroxide gives 10,11-dithia-5H,16H-5,16-diazadinaphtho[2,3a],[2,3c]-1,4-naphtho-quinone-10,11-dioxide 14 which absorbs infrared light at 827nm. The reaction of 1a with 2-aminoethanethiol gives 5-hydroxy-6-chloro-7-thia-10-aza-8, 9,10-trihydrobenzo[2,3a]-1,4-naphthoquinone 4 and 2,3-di-chloro-5-hydroxy-7-thia-10-aza-8, 9,10-trihydrobenzo[2,3a]-1,4-naphtho-quinone 5 in yields of 14.2 % and 3.2 %, respectively. 相似文献
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M. Mühlstdt J. Heinicke A. Seifert M. Rack 《Advanced Synthesis \u0026amp; Catalysis》1995,337(1):283-291
Investigations on the Chemistry of 3-Chloromethyl-3-methyl-2,3-dihydro-1,4-benzoxathiines A series of 3-chloromethyl-2,3-dihydro-1,4-benzoxathiines 3 were prepared by the reaction of several β-methallylphenylethers 1 with sulfur dichloride. In some cases intermediate sulfenyl chlorides 2 were isolated and characterized as substituted thiazolidin-2-ones. The thermal regioisomerization of selected sulfenyl chlorides and one of the thiazolidinone products was achieved. Starting from 3-chloromethyl-2,3-dihydro-1,4-benzoxathiine 3o several derivatives were obtained by nucleophilic displacement at the 3-chloromethyl position, activated by S-3-neighboring group partizipation. The structure of the 3-acetoxymethyl derivative was determined by x-ray crystal structure analysis. Further special derivation with selected chiral reagents led to diastereomeric compounds. The separation of the diastereomers by crystallization and chromatography was attempted. HPLC-separation was achieved in one case. 相似文献
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Díaz-Gavilán M Conejo-García A Cruz-López O Núñez MC Choquesillo-Lazarte D González-Pérez JM Rodríguez-Serrano F Marchal JA Aránega A Gallo MA Espinosa A Campos JM 《ChemMedChem》2008,3(1):127-135
A series of eleven 2- and 6-substituted (R,S)-9-(2,3-dihydro-1,4-benzoxathiin-3-ylmethyl)-9H-purine derivatives was obtained by applying a standard Mitsunobu protocol that led to a six-membered ring contraction from (R,S)-3,4-dihydro-2H-1,5-benzoxathiepin-3-ol via an episulfonium intermediate. The signal approximately delta=151 ppm, which corresponds to the C4' carbon atom, is unequivocal proof of the N9' regioisomer. The potential of the target molecules as anticancer agents is reflected in their activity against the MCF-7 cancer cell line. The most active compounds have IC(50) values of (6.18+/-1.70) and (8.97+/-0.83) microM. The results indicate that the anticancer activity for the most active compounds is correlated with their capacity to induce apoptosis. 相似文献
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建立了反相高效液相色谱法测定农药中间体3-二氟甲基-1-甲基-1H-吡唑-4-甲酸和3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯含量方法.甲醇和20 mmol/L乙酸铵(pH 5.0)为流动相,采用HC-C18色谱柱,在波长240 nm处检测.该方法在12.387~1238.7 mg/L 3-二氟甲基-1-甲基-1H... 相似文献