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以2-氯-5-硝基吡啶为原料,经甲氧基化反应得2-甲氧基-5-硝基吡啶(2),2再与液氨/高锰酸钾进行氨化反应制得2-氨基-6-甲氧基-3-硝基吡啶,总收率77%。 相似文献
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4-喹诺酮-2-羧酸甲酯衍生物的制备,一般是用苯胺衍生物与丁炔二酸二甲酯反应,生成α-(取代苯胺基)丁烯二酸二甲酯(1),继之在二苯醚中约260℃加热环合而获得。我们用间氨基苯酚与丁炔二酸二甲酯在甲醇中反应,所得黄色固体经鉴定为7-羟基-4-喹诺酮-2-羧酸甲酯(2);除去固体后的滤液在甲醇-盐酸中回流还能生成2。若用间苯二胺与丁炔二酸二甲酯反应,则生成7-氨基-4-喹诺酮-2-羧酸甲酯(3)(产率20%)和N,N′-二(1,2-双-甲氧羰基乙烯基)间苯二胺(4)(产率4.8%)。这样就不需要再在二苯醚中进行环合。2与3的易于制备,显示氨基和羟基的活化作用。2和3在室温分别与醋酐-吡啶反应,可得乙酰化物5和6.2和3在二甲基甲酰胺中与乙氧草酰氯(ethyloxalyl chloride)反应,可分别生成化合物7和8。 相似文献
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3,3,6,6-四甲基-9-对氯苯基-1,8-二氧代-2,3,4,5,6,7-六氢氧杂蒽的合成和晶体结构 总被引:2,自引:0,他引:2
标题化合物C2 3H2 5O3Cl是由对氯苯甲醛与 5,5 二甲基 1 ,3环己二酮在乙二醇中反应而得。结构通过单晶X 射线衍射法测定 ,其晶体属于单斜晶系 ,空间群P2 1 /n ,a =6.0 4 8(1 ) ,b =1 9.543(3) ,c =1 7.42 0 (3) ,β =97.2 9(1 )° ,V =2 0 4 2 .2 (6) 3,Mr=384.90 ,Dc=1 2 52 g/cm3,Z =4,μ(MoKα) =2 .0 6cm- 1 ,F(0 0 0 ) =81 6。晶体结构用直接法解出 ,经用全矩阵最小二乘法对原子参数进行修正 ,最终的偏离因子为R =0 .0 39,Rw=0 .0 4 7。X 射线衍射分析表明 :平面 1 (C(8) -C(9) -C(1 9) )与平面 2 (C(1 0 ) -C(1 1 ) -C(1 2 ) )之间的两面角为1 6.2 4° ;平面 1与平面 3(C(7) -C(8) -C(9) )之间的两面角为 1 77.37° ;平面 1与平面 4(C(1 )-C(5) -C(6) )之间的两面角为 98.2 1°;平面 2与平面 3之间的两面角为 1 61 .1 2° ;平面 2与平面 4之间的两面角为 81 .98°;平面 3与平面 4之间的两面角为 79.1 5° 相似文献
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标题化合物C18H21NO5是由2-呋喃亚甲叉氰乙酸酯和5,5-二甲基-1,3-环己酮在醋酸铵存在下用微波辐射反应得到,结构通过单晶X-射线衍射法确定,其晶体属三斜晶系,空间群P 睿琈r =332.36,a =11.232(2),b =13.048(2),c =13.274(3),α=105.7(1),β=95.68(2),g =109.56(1)? V=1752.4(6)3,Z=2,Dc=1.276Mg·m-1, =0.093mm-1,F(000)=704, 最终的偏离因子为R=0.0431,wR=0.0973,在分子结构中平面 1 (呋喃环) 与平面2 ((C(5)、 C(6)、C(9)、O(1))之间的二面角为 84.70°, 平面2 与平面 3 (C(1)、C(4)、C(5)、C(6)) 之间的二面角为 2.9°, 平面 1 与平面3 之间的二面角为 85.9°。吡喃环和与吡喃环合的六员环为信封式结构。 相似文献
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标题化合物C18H18N2O2是由亚苄基丙二睛和5,5-二甲基-1,3-环己酮在乙二醇中反应2小时得到,结构通过单晶X-射线衍射法确定,其晶体属单斜晶系,空间群P21/c,Mr=294.34,a = 11.3070(1), b= 9.4750(1),c = 14.919(2) ,β= 99.34(1)埃琕 = 1577.1(3) 3,Z = 4,Dc=1.240Mgm-3,μ=0.082mm-1,F(000)=624, 最终的偏离因子为R=0.0381,wR=0.0961,在分子结构中存在3个环:苯环(A)、吡喃环(B)及与吡喃环稠合的六员环(C)。A与B、A与C及B与C之间的两面角分别为 92.5°、85.7°和8.2°。 相似文献
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研究了新显色剂1-羟基-2-(5-NO2-2-吡啶偶氮)-8-氨基-3,6-萘二磺酸(简称5-NO2-PAH)与牛血清白蛋白(BSA)的显色反应,建立了5-NO2-PAH光度法测定血清蛋白的新方法.结果表明,在pH 3.0的B-R缓冲液中,牛血清白蛋白与5-NO2-PAH定量络合,导致5-NO2-PAH在530 nm处的吸收降低,且吸光度降低值与BSA量在6~31 μg/mL范围内呈线性关系,摩尔吸光系数为2.2×105 L*mol-1*cm-1,方法检出限为9.8×10-8 mol/L.用摩尔比法测得结合数为130. 相似文献
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4-硝基苯甲酰肼与芳醛反应得到相应的酰腙(2),2与丙酸酐脱水环化合成了标题化合物,其结构经^1H NMR,IR,MS和元素分析表征。 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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Denisova E. I. Lipin D. V. Parkhoma K. Yu. Devyatkin I. O. Shipilovskikh D. A. Chashchina S. V. Makhmudov R. R. Igidov N. M. Shipilovskikh S. A. 《Russian Journal of Organic Chemistry》2021,57(12):1955-1960
Russian Journal of Organic Chemistry - New substituted 2-[2-(4-nitrobenzoyl)hydrazinylidene]-4-oxobut-2-enoic acids have been synthesized by condensation of 4-nitrobenzohydrazide with... 相似文献
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Sulfinylation of o-nitrobenzamide and subsequent hetero Diels-Alder reaction gave a series of 2-(o-nitrobenzoyl)-1,2-thiazine-1-oxides. The 2-(o-nitrobenzoyl)-1,2-thiazine-1-oxides undergo a ring opening reaction with phenyl magnesium bromide to give allylic sulfoxides, which, after [2,3]-sigmatropic rearrangement and desulfurisation, furnish unsaturated vicinal N-(o-nitrobenzoyl)-1,2-amino alcohols. Oxidation of the alcohol and reductive ring closure gave a series of bicyclic 1,2,3,4-tetrahydro-1,4-benzodiazepin-5-ones, a subset of the ‘privileged’ 1,4-benzodiazepine structure. A 4-hydroxy-1,2,5-benzothiadiazepin-1,1-dioxide was synthesised by the same route starting from o-nitrobenzenesulfonamide. 相似文献
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Salvatore Plescia Giuseppe Daidone Maria L. Bajardi 《Journal of heterocyclic chemistry》1982,19(3):685-687
By reaction of some 4-carbethoxy(or cyano)-3(5)-R-5(3)-aminopyrazoles 1 with 2-nitrobenzoyl chloride or 2-nitrobenzenesulfonyl chloride, a number of novel 3- and 5-amino-1-(2-nitrobenzoyl or 2-nitrobenzene-sulfonyl)pyrazoles 6 and 7 were obtained. Every compound appearing during the endocyclic N-substitution process can be identified and determined by glc. The use of nmr offers a rapid, unambigous method for determining the proposed structures. 相似文献
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P. De Caprariis G. De Martino E. Abignente A. Sacchi 《Journal of heterocyclic chemistry》1990,27(3):699-701
Catalytic hydrogenation of 4-acetyl-2,2-dicthoxycarbonyl-2,3-dihydro-1-(2-nitrobenzoyl)pyrrole 2 afforded 3-acetyl-1,1-diethoxycarbonyl-1,2,3,3a,4,9-hexahydro-9-oxopyrrolo[2,1-b]quinazoline 3 and the 4-hydroxy derivative 4 , together with two tetrahydro analogs 5 and 6 of 3 . Compounds 5 and 6 were also obtained by dehydration of 4 . 相似文献
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合成了两个N,N′-取代的靛蓝染料,反式-N,N′-双对硝基苯甲酰基靛蓝(1)和反式N,N′-双间硝基苯甲酰基靛蓝(Ⅱ)。研究了这两个染料与电子给体(胺类化合物)或与电子受体(紫精化合物)之间的电子转移。结果表明,这两个染料在激发单重态经荧光猝灭,被紫精猝灭的速度常数(kq)比被胺猝灭的速度常数大。 相似文献
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M. Srinivasan J. B. Rampal S. Thiagarajan 《Phosphorus, sulfur, and silicon and the related elements》2013,188(2):221-226
Abstract A comparative electron impact study on 2-(2′-nitrobenzoyl)thiophene1(1), 2-(2′-nitrobenzoyl)-3-methylthiophene2(2) and the corresponding 4′-nitrobenzoyl derivatives (3 and 4)3,4 is presented. The results suggest that the presence of nitro group β-to the carbonyl affects the general fragmentation pattern recorded in the literature for 2-acyl and 2-aroylthiophenes. 相似文献
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V. A. Shkulev I. B. Saakyan Ts. E. Agadzhanyan 《Chemistry of Heterocyclic Compounds》1992,28(11):1340-1345
7-Aroyl- and 7-heteroyl-1,3,5-triazaadamantanes were obtained by condensation of aromatic and heterocyclic compounds containing an acetyl group with hexamethylenetetramine in the presence of acetic acid. Reactions with 7-benzoyl- and 7-(4-nitrobenzoyl)-1,3,5-triazaadamantanes at both the carbonyl group and in the triazaadamantane ring were carried out. Ring-deuterated 7-nitro- and 7-(4-nitrobenzoyl)-1,3,5-triazaadamantanes were synthesized in order to ascertain the pathway of mass-spectrometric fragmentation, as well as a possible mechanism for the construction of the triazaadamantane ring.For Communication 15 see [1].Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 11, pp. 1565–1571, November, 1992. 相似文献
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A high-performance liquid chromatographic method without prederivatization was investigated for the direct determination of 4-nitrobenzoyl chloride and 4-nitrobenzoic acid. The separation was carried out on C3, C8 and C18 alkyl-bonded silica columns with cyclohexane-tetrahydrofuran as the eluent. The retention behaviour observed was obviously caused by the silanophilic interaction between the solute and stationary phase. Optimum separation of 4-nitrobenzoyl chloride and 4-nitrobenzoic acid was obtained on the C3 column and the calibration graph showed a significant linear relationship. The method was found to be quantitative, reproducible and rapid. 相似文献