Synthesis and Crystal Structure of Ethyl 3-（4-Chlorophenyl）-3,4-dihydro-6-methyl-4-oxo-2- （pyrrolidin-1-yl）furo[2,3-d]pyrimidine-5-carboxylate

The crystal structure of the title compound ethyl 3-（4-chlorophenyl）-3,4-dihydro-6- methyl-4-oxo-2-（pyrrolidin-1-yl）furo[2,3-d]pyrimidine-5-carboxylate （C20H20ClN3O4, Mr= 401.84） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215（9）, b = 8.5311（4）, c = 21.6886（9） A^°, β = 91.607（1）°, V = 3814.0（3）A^°^3, Z = 8, Dc = 1.400 g/cm^3, F（000） = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.     

Interaction of 1-Benzyl-4-benzoyl-5-phenyl-2,3-dihydro-2,3-pyrroledione with Ketene Diethylacetal: Synthesis and Crystal and Molecular Structure of 1-Benzyl-4-benzoyl-3-hydroxy-5-phenyl-5-ethoxycarbonylmethyl-2,5-dihydro-2-pyrrolone

1-Benzyl-4-benzoyl-5-phenyl-2,3-dihydro-2,3-pyrroledione reacts with ketene diethylacetal, forming 1-benzyl-4-benzoyl-3-hydroxy-5-phenyl-5-ethoxycarbonylmethyl-2,5-dihydro-2-pyrrolone, whose crystal and molecular structure was studied by XRD.     

Synthesis of 5-[2-(Phenoxy)ethyl] Derivatives of 6-Methyluracil, 6-Methyl-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one,and 2-Imino-6-methyl-2,3-dihydro-1H-pyrimidin-4-one

A synthesis of novel derivatives of 6-methyluracil, 6-methyl-2-thioxo-, and 2-imino-6-methyl-2,3-dihydro-1H-pyrimidin-4-one containing a 2-(phenoxy)ethyl substituent at position 5 of the pyrimidine ring has been carried out. It was found that 5-[2-(phenoxy)ethyl] derivatives of 6-methyl-2-thioxo- and 2-imino-6-methyl-2,3-dihydro-1H-pyrimidin-4-one are obtained by the condensation of the corresponding ethyl 3-oxo-2-(2-phenoxyethyl)butanoates with thiourea or guanidine. 6-Methyl-5-[2-(phenoxy)ethyl]uracils can be prepared by treating 6-methyl-5-[2-(phenoxy)ethyl]-2-thioxo-2,3-dihydro-1H-pyrimidin-4-ones with an excess of aqueous monochloroacetic acid solution. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 8, pp. 1213–1217, August, 2005.     

Interaction of 5-aryl-4-quinoxalinyl-2,3-dihydro-2,3-furandiones with mesitylamine and methyl(phenyl)hydrazine. Synthesis and crystal and molecular structure of 2-(1-mesityl-4,5-dioxo-2-phenyl-4,5-dihydro-3-pyrollyl)-3-phenylquinoxaline

The interaction of 5-aryl-4-quinoxaline-2,3-dihydro-2,3-furandiones with mesitylamine and methyl(phenyl) hydrazine results in the formation of 1-substituted 5-aryl-4-quinoxalinyl-2,3-dihydro-2,3-pyrrolediones. The crystal and molecular structure of the 1-mesityl-5-phenyl derivative was investigated by X-ray diffraction.Original Russian Text Copyright © 2004 by Z. G. Aliev, N. Yu. Lisovenko, L. O. Atovmyan, and A. N. MaslivetzTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 3, pp. 553–557, May–June 2004.     

4-Hydroxy-2-quinolones. 90. Synthesis and antitubercular activity of 4-methyl-2-thiazolylamides of halo-substituted 4-hydroxy-2-oxo-1,2-dihydro-3-quinolinecarboxylic acids

Several variants were studied for the synthesis of esters of halogen derivatives of 4-hydroxy-2-oxo-1,2-dihydro-3-quinolinecarboxylic acids, whose reaction with 2-amino-4-methylthiazole gives the corresponding hetarylamides. Results are given for a study of the antitubercular activity of these products. Communication 89, see ref. [1]. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 71–76, January, 2006.     

6-芳甲氧基-7-甲基-4-羟基-3-喹啉羧酸乙酯类化合物的合成及抗球虫活性研究

本文通过亚硝化、催化氢化、EMME缩合、醚化和关环五步反应合成了3个未见文献报道的6-芳甲氧基-7-甲基-4-羟基-3-喹啉羧酸乙酯类化合物。所有化合物的结构均经1H NMR,IR和HRMS等方法确证。对三个化合物进行了抗球虫活性实验,实验结果表明,在27 mg/kg的使用浓度下,化合物6-苄氧基-7-甲基-4-羟基-3-喹啉羧酸乙酯(5a)具有抗球虫活性。     

4-Hydroxy-2-quinolones 120. Synthesis and structure of ethyl 2-hydroxy-4-oxo-4H-pyrido-[1,2-a]pyrimidine-3-carboxylate

An improved method for the preparation and purification of ethyl 2-hydroxy-4-oxo-4H-pyrido[1,2-a]-pyrimidine-3-carboxylates is proposed. According to ¹H and ¹³C NMR spectroscopic data the synthesized compounds exist in DMSO solution in the 2-hydroxy-4-oxo form while in the crystal (at least for the case of the unsubstituted derivative) X-ray analysis shows that it occurs in the bipolar 2,4-dioxo form. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 864–876, June, 2007.     

Nucleophilic reactions of 1-methyl-2-methoxy-2-phenyl-3-oxo-2,3-dihydroindole

The title compound (1) was prepared via methylene blue (MB)-sensitized photooxy-genation of l-methyl-2-phenylindole (2d) in methanol. Acid-catalyzed nucleophilic substitution of 1 with nucleophiles gave 1,2,2-trisubstituted 3-oxo-2,3-dihydroindoles (3-6). Reduction of 1 with lithium aluminum hydride, followed by acidic workup yielded 4d and 2d, whereas the same reduction reaction of 1, followed by neutral workup gave l-methyl-2-phenyl-3-hydroxy-2,3-dihydroindole (15), together with 3. The reaction pathways of nucleophilic substitution and reduction of 1 were discussed.     

4-双(1-苯基-3-甲基-4-吡唑啉-5-酮)甲烷的晶体结构

杂环化合物1 苯基 3 甲基 4 吡唑啉 5 酮(ＨＰＭＰ)为β 二酮,不仅可用作金属离子的萃取剂,还可用于核磁共振的位移试剂,也可用于激光、催化、生化、医学等领域[1-4]。我们从ＰＭＰ出发,合成了它的Ｃｏ(Ⅱ),Ｎｉ(Ⅱ),Ｃｕ(Ⅱ)和Ｚｎ(Ⅱ)的络合物[5,6]。利用单晶Ｘ 射线衍射分析方法报道了标题化合物的晶体结构。1　实验部分在合成ＰＭＰ席夫碱化合物的过程中,得到标题化合物的单晶体。元素分析结果(括号内为计算值)Ｃ%:69 87(69 98),Ｈ%:5 62(5 59),Ｎ:15 61(15 55)。红外光谱(ＫＢｒ):1645和1637ｃｍ-1的强吸收峰归属为羰基的伸缩振动,…     

4-hydroxy-2-quinolones. 153*. Synthesis of hetarylamides of 4-methyl-2-oxo-1,2-dihydroquinoline-3-carboxylic acid

4-Methyl-2-oxo-1,2-dihydroquinoline-3-carboxylic acid hetarylamides can be prepared by two fundamentally different routes with allowance made for the thermal stability of the starting hetarylamines. * For Communication 152 see [1]. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 3, pp. 426–432, March, 2009.     

4-Hydroxyquinolones-2. 91. Synthesis and properties of ethyl 1-R-4-hydroxy-6-methyl-2-oxo-dihydropyridine-5-carboxylates

The reaction of ethyl aminocrotonates with derivatives of malonic acid is a suitable method for the preparation of ethyl 4-hydroxy-6-methyl-2-oxo-1,2-dihydropyridine-5-carboxylates. One of the synthesized materials has been studied by X-ray crystallography. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 2, 217–223, February, 2006.     

Dehydration of 4-hydroxy-4-methyl-3-phenylamino-oxazolidin-2-ones

The dehydration of two 5,5-disubstituted 4-hydroxy-4-methyl-3-phenylaminooxazolidin-2-ones into the corresponding 4-methylene-3-phenylaminooxazolidin-2-ones has been carried out. The structure of the products was confirmed by X-ray diffraction analysis.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1512–1517, October, 2004.     

Nucleophilic reactions of l-methyl-2-methoxy-2-phenyl-3-oxo-2,3-dihydroindole

The title compound (1) was prepared via methylene blue (MB)-sensitized photooxy-genation of l-methyl-2-phenylindole (2d) in methanol. Acid-catalyzed nucleophilic substitution of 1 with nucleophiles gave 1,2,2-trisubstituted 3-oxo-2,3-dihydroindoles (3–6). Reduction of 1 with lithium aluminum hydride, followed by acidic workup yielded 4d and 2d, whereas the same reduction reaction of 1, followed by neutral workup gave l-methyl-2-phenyl-3-hydroxy-2,3-dihydroindole (15), together with 3. The reaction pathways of nucleophilic substitution and reduction of 1 were discussed.     

Synthesis of fused pyran and arylbis（4-hydroxy-6-methyl-2-oxo-2H-pyran-3-yl）methane in ionic liquid

Promoted and mediated by an ionic liquid-[bmim][BF4].fused pyrans or arylbis(4-hydroxy-6-methyl-2-oxo-2H-pyran-3-yl)methanes were efficiently and selectively prepared from the reaction of aldehyde and 4-hydroxy-6-methyl-2-oxo-pyran with or Without acetic anhydride.By using these novel procedures,pyrimidine nucleoside-fused pyran and arylbis(pyranon-3-yl)methane hybrids with potential biological activities were constructed.     

Crystal structures of ethyl-4-(5-bromo-2-hydroxyphenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate and ethyl-1-methyl-15-oxo-2-oxa-14,16-diazatetracyclo [11.3.1.0<Superscript>3.12</Superscript>.0<Superscript>6.11</Superscript>]heptadeca-3,5,7,9,11-pentaene-17-carboxylate

The crystal structures of ethyl-4-(5-bromo-2-hydroxyphenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate and ethyl-1-methyl-15-oxo-2-oxa-14,16-diazatetracyclo[11.3.1.0^3.12.0^6.11]heptadeca-3,5,7, 9,11-pentaene-17-carboxylate were determined by XRD, and the conformations of their structures were determined.     

Interaction of 4,5-diphenyl-2,3-dihydro-2,3-pyrroledione with ethoxycarbonylmethylenetriphenylphosphorane: synthesis and crystal structure of 4,5-diphenyl-Z-2-ethoxycarbonylmethylene-2,3-dihydro-3-pyrrolone

1-Unsubstituted 4,5-diphenyl-2,3-dihydro-2,3-pyrroledione interacts with ethoxycarbonyl-methylenetriphenylphosphorane regioselectively to give 4,5-diphenyl-Z-2-ethoxycarbonyl-methylene-2,3-dihydro-3-pyrrolone. The crystal and molecular structure of the latter was studied by X-ray analysis.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1556–1558, August, 1995.