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The title compound (C22H27NO3) was obtained by the reaction of 4-methylbenzal- dehyde, dimedone, ethyl acetoacetate and ammonium acetate in water in the presence of triethyl- benzylammonium chloride (TEBA). The crystal is of orthorhombic, space group Pbcn with a = 18.242(2), b = 15.651(1), c = 14.207(2) (A), V = 4056.15(64) (A)3, Mr = 353.45, Z = 8, Dc = 1.158 g/cm3, μ = 0.076, λ(MoKα) = 0.71073 (A) and F(000) = 1520. The final R = 0.0453 and wR = 0.0436 for 1156 observed reflections with I > 2((Ⅰ). X-ray analysis revealed that the pyridine ring is of boat conformation and the six-member ring fused with it adopts half-chair conformation. 相似文献
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1 INTRODUCTION The 1,4-dihydropyridines (1,4-DHPs) are biologi- cally interesting compounds and have been developed extensively in pharmacology. 1,4-DHP derivatives are used therapeutically in the treatment of cardio- vascular disorders, especially hypertension and coro- nary heart disease such as angina pectoris, atheros- clerosis, etc. The DHPs have emerged as one of the most important classes of drugs for the treatment of gastrointestinal disease, Raynaud?s disease, pulmonary hyper… 相似文献
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The reaction of dimedone, N-aryl-substituted acetoacetic acid amides, aryl aldehydes, and ammonium acetate gives 4,N-diaryl-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydro-3-quinoline carboxamides. 相似文献
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微波辐射下2,7,7-三甲基-3-乙氧羰基-4-(3-硝基苯基) -5-氧代-1,4,5,6,7,8-六氢喹啉的合成和晶体结构 总被引:2,自引:0,他引:2
标题化合物C21H24N2O5是由间硝基苯甲醛、达咪酮、乙酰乙酸乙酯、醋酸铵在微波辐射下干反应而得。结构通过单晶X-射线衍射法确定,其晶体属斜方晶系,空间群 Pbcn, a =17.953(3), b =15.206(4), c =14.299(3), V =3904.(2)3, Mr =384.42, Z =8, Dc =1.308g/cm3 , m(MoKa) =0.094mm-1, F(000)=1632。晶体结构用直接法解出,经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=0.0493, wR=0.1078。X-射线分析结果表明,吡啶环为船式构象,与之稠合的六元环为信封式构象。 相似文献
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报道了用3-甲酰基色酮、5,5-二甲基-1,3-环己二酮、乙酰乙酸乙酯与醋酸铵一步法合成4-(色酮-3-基)-3-乙氧羰基-1,4,5,6,7,8-六氢-5-氧代-2,7,7-三甲基喹啉类化合物, 对其结构进行了表征, 并分析了代表性化合物2f的晶体结构. 2f晶体属于单斜晶系, P2/c空间群, 所得晶胞参数为: a=2.0255(4) nm, b=0.9132(2) nm, c=1.4066(3) nm, β=121.60(3)°, V=2.2159(8) nm3, Z=4, Dc=1.335 g/cm3, μ=0.209 mm-1, F(000)=736, R1=0.0556, wR2=0.1248. 相似文献
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V. L. Gein M. I. Kazantseva L. F. Gein P. A. Slepukhin 《Russian Journal of Organic Chemistry》2014,50(2):240-243
Reactions of alkyl acetoacetates, aromatic aldehydes, ammonium acetate, and 1,3-cyclohexanedione afford alkyl 4-aryl-2-methyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylates. The structure of compounds obtained was established with the help of IR, 1H NMR, and mass spectra and by X-ray diffraction analysis. 相似文献
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S. G. Krivokolysko V. D. Dyachenko V. P. Litvinov 《Chemistry of Heterocyclic Compounds》1999,35(2):206-207
By reaction of isovaleric aldehyde with cyanothioacetamide and cyclohexane-1,3-dione, 3-cyano-4-isobutyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-1-thiol has been obtained, and subsequently used in synthesis of the corresponding substituted 2-alkylthiohexahydroquinolines.Lugansk T. G. Shevchenko State Pedagogical Institute, Lugansk 348011, Ukraine. N. D. Zelinskii Institute of Organic Chemistry, Russian Academy of Sciences, Moscow 117913, Russia. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 2, pp. 230–231, February, 1999. 相似文献
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Ali Souldozi Seyed Hamid Reza Shojaei Ali Ramazani Katarzyna lepokura Tadeusz Lis 《结构化学》2013,32(1):82-88
The title compound, methyl 2-(diphenylamino)-4-phenyl-1,3-thiazole-5-carboxylate, was synthesized and studied by single-crystal X-ray diffraction method. The structure of the product was confirmed by IR, 1H- and 13C-NMR spectroscopy and elemental analysis. These experimental studies were supported by quantum mechanical calculations. The structure was solved in monoclinic, space group P21/c with a = 9.573(3), b = 19.533(7), c = 9.876(3), β = 92.35(4)°, V = 1845.2(10)3, T = 85(2) K, Z = 4, R = 0.040 and wR = 0.089 for 6424 observed reflections withI>2σ(I). 相似文献
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1INThODUCT1ONInaprevi0uspaPer"',wereP0rtedthesyntheses0fsome1,3,4-diazaphospho-lidin-2-thione-4-oxidesandtheirhighselectiveherbicidalactivity.Althoughtherewereseveralreportsaboutthedesulphurisationofsomestraightchainthioureaderiva-tivest2'31,uptonow,thedesulphurisationreactionofcyclicthioureaderivativesutiliz-ingAgNO,-H,Osystemhasnotbeenstudied.InthispaPer,thedesulphurisation0fcis-3,4-diphenyl-5-(2,4-dichlorophenyl)-1,3,4-diazaphOSpholidin-2-thione-4-oasthecyclicsubstrateisrep0rtedfort… 相似文献
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The compound (Z)-ethyl 5-(phenylamino)-3-(phenylimino)-3H-1,2-dithiole-4-carboxylate 3 has been synthesized by the reaction of ethylacetoacetate 1 and phenylisothiocyanate 2. Its structure has been established by 1H NMR, 13C NMR, infrared, mass spectra, and x-ray crystallography. 相似文献
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<正>The crystal structure of the title compound (C16H17NO5) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group C2/c with a = 18.520(2), b = 7.8910(1), c = 21.728(3) A, β = 104.77(1)°, V= 3070.4(7) A3, Mr= 303.31, Z = 8, Dc= 1.312 g/cm3, λ = 0.71073 A,μ(MoKα) = 0.098 mm-1 and F(000) = 1280. The structure was refined to R = 0.0486 and wR = 0.1287. There exist intermolecular hydrogen bonds in the crystal. 相似文献
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De-Jian Wang Qiong-Lin Mou Shi-Guan Wan Xin-Jian Song Da-Ting Tian 《Phosphorus, sulfur, and silicon and the related elements》2013,188(8):944-951
Abstract 2-(3-Silatranylpropylamino)-4-(2,4-dichlorophenyl)-5,5-dimethyl-1,3,2-dioxa phosphinane-2-sulfide 4 was synthesized by a nucleophilic substitution reaction of 2-chloro-1,3,2-dioxaphosphinane-2-sulfide 2 with γ-aminopropylsilatrane 3, which was prepared by the cyclization reaction of triethanolamine and γ-aminopropyltriethoxysilane. The structure of the title compound was confirmed by IR, 1H NMR, 31P NMR, EI-MS, and elemental analysis as well as by single crystal X-ray diffraction and its thermal properties were studied by thermogravimetry (TG) and differential scanning calorimetry (DSC). Thermal analysis and preliminary fire retardance testing suggest that compound 4 should function as a good flame retardant. 相似文献