2-硫代-4-咪唑啉二酮的合成与表征

咪唑啉酮衍生物是一类线粒体呼吸抑制剂,对果树黑斑病及由卵菌引起的霜霉病、疫病等的活性很好。2-硫代-5-苯基亚甲基4-咪唑啉二酮衍生物不能用通法制取,其起始原料烯基氨基酸不稳定。本文用三组分串联aza-Wittig堍反应合成2-硫代-3-烷基-5-苯基亚甲基4-咪唑啉二酮类化合物。合成路线如下：     

2-烷硫基-5-苯基亚甲基-4H-咪唑啉-4-酮的合成与表征

用2-硫代-3-正丁基-5-苯基亚甲基4-咪唑啉二酮的-S-烷基化反应合成了2-烷硫基-3-正丁基-5-苯基亚甲基-4H-咪唑啉-4-酮衍生物。探讨了S-烷基化反应的反应条件和所合成化合物的波谱性质。目标产物均为新的化合物，其结构经元素分析，IR，1H NMR和MS确正。     

荧光试剂3-苯基-5-苯甲酰基-2-硫代-4-噻唑啉酮的合成及应用

本文报道了荣光试剂3-苯基-5-苯甲酰基-2-疏代-4-噻唑啉酮（PBTT）的合成。产品经拉层桥提纯，用元素分析、IR、1HNMR和MS确证了其结构；研究了它的荧光性质。在PH5．6时，与痕量镜（Ⅲ）形成络合物。且在λex/λem=305nm／405nm产生强荧光。测定了人工合成样品中的铥，结果比较满意。     

3—芳基—5—苯甲酰基—2—硫代—4—噻唑啉酮的合成

报道了３－芳基－２－硫代－４－噻唑啉酮和３－芳基－５－苯甲酰基－２－硫代－４－噻唑啉酮系列化合物的合成，其中１１种化合物示见文献报道。结构经元素分析，红外光谱，核磁共振氢谱和质谱确证，讨论了合成反尖条件下和质谱裂解途径，初步生理活性试验结果表明，２ｄ和２ｅ具有一定的生理活性。     

1,3-二甲基-2-咪唑啉酮的纯度测定

建立了一种简便、准确的测定1,3-二甲基-2-咪唑啉酮纯度的气相色谱分析方法,通过对反应过程中产物的跟踪测试,指导合成,使其产品纯度达到99.9%以上.     

2-(4-甲硫基苯氧基)－4H－咪唑啉-4-酮衍生物的合成及生物活性

咪唑啉酮;2-(4-甲硫基苯氧基)－4H－咪唑啉-4-酮衍生物的合成及生物活性     

2-硫代-3-烷基-5-苯基亚甲基-4-咪唑啉二酮衍生物的有效合成新方法

应用烯基膦亚胺与二硫化碳、一级脂肪胺的串联aza-Wittig反应合成了2-硫代-3-烷基-5-苯基亚甲基-4-咪唑啉二酮衍生物。提出了可能的环化反应机理，探讨了所合成化合物的成环反应条件和波谱性质。经元素分析、IR,1H NMR和MS确证产物均为新化合物。     

壳聚糖-g-N-羧甲基-2-硫代-4，5-2H咪唑啉酮的制备及其抑菌性能

以2-溴乙酸、壳聚糖、2-硫代四氢咪唑啉酮为原料,合成了不同接枝率的壳聚糖-g-N-羧甲基-2-硫代-4,5-2H咪唑啉酮（CTS-g-CSIDZ）,并对其理化性质进行了考察。用络合滴定法测定了该聚合物对Cd²⁺,CrO4^2-,Fe³⁺,Cu²⁺,Pb²⁺等重金属离子的吸附作用;进行了聚合物的悬菌定量实验,测定了接枝聚合物对一系列细菌的抑制能力;采用失重法研究了合成的聚合物在1mol/L HCl溶液中对N80钢片腐蚀的抑制作用。结果表明,部分接枝的CSIDZ比小分子化合物具有更高的对测试的多数金属离子吸附作用的热稳定性;接枝CSIDZ具有较强的抑菌效果,最小抑菌浓度为5.10 g/L;接枝CSIDZ比小分子缓蚀剂具有更高的热稳定性,在90 ℃时对N80钢片的缓蚀效率仍然可以达到71.1％,且用量仅为小分子化合物CSIDZ的1/2。     

咪唑啉酮胺类衍生物的合成

咪唑啉酮胺类衍生物的合成;咪唑啉二酮;4H-咪唑啉酮;aza-Wittig反应;合成     

2-氨基-4H-咪唑啉-4-酮衍生物的快速平行合成法

咪唑啉酮衍生物是一类具有良好生物活性和药理活性的杂环化合物 [1,2 ] ,尤其是一些 2 -氨基咪唑啉酮表现出良好的杀菌、抗炎及抗癌活性 [3 ,4 ] .从自然界如一些海洋生物中可分离得到含 2 -氨基咪唑啉酮结构的生物碱 [5,6] .最近 ,组合化学方法广泛地应用于有机合成 ,它包括固相合成法和液相合成法[7～ 9] .我们曾应用氮杂 Wittig反应制得 2 -氨基取代咪唑啉酮衍生物 ,部分化合物表现出一定的抑菌活性 [10 ,11] .本文进一步报道应用液相平行反应法快速合成 2 -氨基 - 4H-咪唑啉 - 4-酮衍生物 (4) .该方法应用烯基膦亚胺 1与苯基异氰酸酯的…     

Synthesis of 2-thioxo-1,3-thiazolidin-4-one derivatives

A series of new 2-thioxo-1,3-thiazolidin-4-one derivatives containing arylidene, arylazo, and aminomethylene fragments in position 5 of the rhodanine cycle was synthesized. Dedicated to Academician V. A. Tartakovsky on the occasion of his 75th birthday. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1564–1569, August, 2007.     

Multicomponent Synthesis of 2,5-Dioxo- and 4-Aryl-5-oxo-2-thioxo-1,2,3,4,5,6,7,8-octahydroquinazolines

Ten 2,5-dioxo- and 4-aryl-5-oxo-2-thioxo-1,2,3,4,5,6,7,8-octahydroquinazolines have been synthesized in three-component interactions of 1,3-cyclohexanedione or dimedone, urea or thiourea, and substituted benzaldehydes (3-bromo-, 4-bromo-, 4-fluoro-, 4-methoxy-, 3,4-methylenedioxy-, and 3-nitro-). 9-Aryl-4,5-dioxo-1,2,3,4,5,6,7,8-octahydro-9H-xanthenes were also formed in these reactions.     

Facile Synthesis of Some New Pyrazole-Based 2-Thioxo-4-thiazolidinone

5-Ethoxymethylene-2-thioxo-4-thiazolidinone (1) reacts with hydrazine hydrate at room temperature to afford 5-(hydrazinylmethylene)-2-thioxo-4-thiazolidinone (3). Compound 3 condensed with different aromatic aldehydes 6a–d in ethanol in the presence of a few drops of piperidine to give the corresponding Schiff’s bases 7a–d. On the other hand, compound 3 reacts with o-hydroxybenzaldehyde derivatives 8a and 8b in refluxing ethanol catalyzed by a few drops of piperidine to yield 1H-inadzolyl-2-thioxo-4-thiazolidinones 9a and 9b. Reaction of compound 3 with α-ketoesters 10a and 10b or α-diketones 10c–e in refluxing glacial acetic acid furnished the pyrazolyl-2-thioxo-4-thiazolidinone derivatives 11a–e. Also, compound 3 reacts with some different enaminones 12a–f in refluxing glacial acetic acid to afford the new pyrazolyl-2-thioxo-4-thiazolidinone derivatives 13a–f. Pyrazoles 15a–d was obtained via reaction of compound 3 with chalcones 14a–d in dimethylformamide (DMF). The structures of all the newly synthesized products were confirmed on the basis of their elemental and spectral data, and a plausible mechanism has been postulated to account for their formation.     

Solvent Free One-Pot Synthesis of 2-thioxo-1,3-thiazinane-4-one Derivatives

Abstract

An efficient one-pot synthesis of 2-thioxo-1,3-thiazinane-4-one derivatives through the reaction of primary amines and carbon disulfide in the presence of acryloyl chloride is described. This reaction is carried out under solvent-free condition and without any catalyst at room temperature within 15 min. The structures of products were deduced from their elemental analysis and IR, ¹H NMR, and ¹³C NMR spectroscopy, and mass spectrometric data.

[Supplementary materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfer, and Silicon and the Related Elements for the following free supplemental files: Additional figures.]     

5-Arylmethylene-2,4-imidazolidinediones and 5-arylmethylene-2-thioxo-4-imidazolidinones derivatives: stereochemistry elucidation by H and C NMR

Derivatives of 5-arylmethylene-2,4-imidazolidinediones and 5-arylmethylene-2-thioxo-4-imidazolidinones were synthesized as potential aldose reductase inhibitors (ARI). The Z/E configuration was elucidated by homonuclear NOE difference spectra and by proton-carbon coupling constant measurement from ¹³C coupled spectra using GATEDEC and SFDEC programs.     

Synthesis and Crystal Structure of 3-Carbamoyl-6-methyl-5-phenylcarbamoyl-2-thioxo-1,2,3,4-tetrahydropyridine-4-spirocyclohexane

3-Carbamoyl-6-methyl-5-phenylcarbamoyl-2-thioxo-1,2,3,4-tetrahydropyridine-4-spirocyclohexane has been synthesized by the condensation of cyclohexylidenecyanothioacetamide with acetoacetanilide and piperidine. The structure of the product was established by X-ray structural analysis.     

Synthesis and Crystal Structure of 4-tert-Butyl-6-（4-chlorophenyl）-3,6- dihydro-2H-1,3-thiazin-2-iminium Chloride

The title compound, 4-tert-butyl-6-（4-chlorophenyl）-3,6-dihydro-2H-1,3-thiazin- 2-iminium chloride （C14H18C12N2S）, has been synthesized by the reaction of 1-（4-chlorophenyl）- 4,4-dimethylpent-1-en-3-one with thiourea, and its crystal structure was determined by single- crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P211c with a = 16.3064（11）, b = 9.4471（6）, c = 11.2626 （8）A, β = 108.400（1）°, Z = 4, V = 1646.28（19） A^3, Mr = 317.26, Dc = 1.280 g/cm^3, S = 1.078,μ = 0.510 mm^-1, F（000） = 664, the final R = 0.0514 and wR = 0.1412 for 3210 observed reflections （I 〉 2σ（I））. The thiazine ring system displays a twisted boat conformation, and three N-H,..Cl hydrogen bonds exist in the crystal. The combination of two N-H...Cl hydrogen bonds generate an R2^1 （6） ring.