Formation and structure of 1-Amino-4-methyl-4-(4-methyl-5-phenyl-1H-pyrazol-3-ylamino)-3-phenyl-4,5-dihydro-1H-pyrazol-5-one

The title compound 3 was obtained during the rearrangement of isoxazol-5-yl hydrazine 1 to 1-aminopyrazolone 2 at 115°. X-ray analysis of the corresponding benzylidene derivative allowed us to achieve the structure assignment.     

2-甲基-4-羟基-6-苯基嘧啶和2-甲基-4-羟基-5-溴-6-苯基嘧啶的高效液相色谱法分离测定

采用ODS-C18色谱柱和紫外检测器,对2-甲基-4-羟基-6-苯基嘧啶和2-甲基-4-羟基-5-溴-6-苯基嘧啶的含量进行HPLC分离测定.以甲醇水=4555为流动相,紫外检测波长为237 nm,样品线性范围为0.001～0.1 mg/mL.2-甲基-4-羟基-6-苯基嘧啶的RSD为0.5%;2-甲基-4-羟基-5-溴-6-苯基嘧啶的RSD为1.0%.     

Synthesis and properties of 1-methyl-2-phenyl-5-(2-furyl)- and 1-methyl-2-phenyl-5-(2-thienyl)imidazoles

2-Phenyl-5-(2-furyl)- and 2-phenyl-5-(2-thienyl)imidazoles were synthesized by condensation of 2-furoylmethyl and 2-thenoylmethyl acetates with benzaldehyde under the conditions of Weidenhagen reaction. The products were converted to N-methyl derivatives in the KOH-acetone system. The electrophilic substitution reactions of the products (acylation, bromination, nitration, sulfonation, hydroxymethylation) were studied.     

1-苯基-5-(3,4-二甲氧基苯基)-3-羟基吡唑的合成和晶体结构

标题化合物(I)是由 1-苯基-5-(3, 4-二甲氧基苯基)-3-吡唑烷酮在 FeCl3催化下被氧气氧化得到的。它的结构经过了元素分析、IR、1H NMR 的表征,用 X-射线衍射法测定了化合物的晶体结构。C17H16N2O3(I)的晶体学参数分别为:三斜晶系,P1空间群,a = 6.6600(13),b = 8.4200(17),c = 14.060(3) ?,α= 85.61(3), β= 76.89(3), γ= 81.18(3)?, Z = 2, Dc= 1.298g/cm3, V = 758.1(3) ?3, Mr = 296.32,μ= 0.090 mm–1, F(000) = 312, R = 0.048,wR = 0.1231。结构测定表明化合物的吡唑环存在着一个大的共轭体系,含有一个稳定的烯醇结构,分子通过分子间的氢键形成了网状的结构。     

Tautomerism of 1-phenyl-3-methyl-4-benzyl-5-pyrazolone

The tautomerism of 1-phenyl-3-methyl-4-benzyl-5-pyrazolone —a side product in the reaction of acetoacetic ester with benzaldehyde phenylhydrazone — was studied by IR and PMR spectroscopy, and its thermodynamic characteristics were determined.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 3, pp. 355–359, March, 1991.     

2,6-双(3-甲基-1-苯基-5-吡唑啉酮-4-基)吡啶二酮的合成

首次通过一步反应合成了2,6-双（3-甲基-1-苯基-5-吡唑啉酮-4-基）吡啶二酮,其结构经1^H NMR,IR和元素分析表征。     

Solvent extraction of gold(III) with 1-phenyl-3-methyl-4-trifluoroacetylpyrazolone-5

A simple, rapid and selective separation procedure of gold based on its extraction with 1-phenyl-3-methyl-4-trifluoroacetylpyrazolone-5 has been developed. The dependence of the distribution ratio of gold on the pH of aqueous solutions, concentration of hydrochloric, nitric and perchloric acids and the organic solvents has been investigated. Decontamination factors for a number of metal ions with respect to gold are reported. Excellent separation of gold is obtained from many elements including noble metals. Citrate, cyanide, iodide, thiosulfate and thiourea completely mask gold, whereas oxalate does not interfere. Solutions of 1 M HCl, 0.2 M KCN, and the buffer of pH 0.8 readily strip gold from the organic phase. Some useful analytical applications of this procedure are discussed.     

Synthesis starting from 3-methyl-2-phenyl-5-(3-methyl-2-phenyl-3,4-dehydropiperidyl-6)pyridine. 2-phenyldinicotinic and 4-azafluorenone-2-carboxylic acids

N-Methyl (ethyl, benzoyl, trifluoroacetyl)-substituted 3-methyl-2-phenyl-5-(3-methyl-2-phenyl-3,4-dehydropiperidyl-6) pyridines and di(N-oxide) of the correspondingly substituted ,ß-dipyridyl were prepared. A method for synthesizing 2-phenyldinicotinic acid was developed. Cyclodehydration of this acid gave 4-azafluorenone-2-carboxylic acid. Transformations of this acid were carried out with respect to two functional groups.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 813–817, June, 1986.     

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,…     

X-ray diffraction and spectral studies of 1-phenyl-3-methyl-4-(2′,4′-Dimethylphenylazo)-pyrazolone-5

The molecular and crystal structures of 1-phenyl-3-methyl-4-(2,4-dimethyl-phenylazo) pyrazolone-5 were determined. In the crystal the molecule exists as the hydrazone tautomer. The pyrazole ring is planar, and the substituents are practically coplanar with it. The molecule contains an intramolecular NH...O hydrogen bond that closes a practically planar six-membered ring (N...O, 2.77 (I), H...O 2.14 Å, angle at H(N(4)) hydrogen 131 °). The x-ray diffraction data agree with the spectral data and with the CNO calculation.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 816–821, June, 1985.     

1-苯基-3-甲基-4-(4-羟基-3-甲氧基)-苯甲叉-吡唑啉酮的微波合成和晶体结构

标题化合物C18H16N2O3是由香草醛和1-苯基-3-甲基-吡唑啉酮用微波辐射反应得到,结构通过单晶X-射线衍射法确定,其晶体属单斜晶系,空间群P21/c,Mr = 308.33, a = 21.101(4), b = 7.984, c = 20.076 ? = 115.81(1)? V = 3044.8(8) ? Z = 8, Dc = 1.345 g/cm3, = 0.093 cm-1, F(000) = 1296, 最终的偏离因子为R = 0.0403, wR = 0.0780, 分子之间存在氢键,形成了网状结构。