卤代-2-(3-甲基-5-取代-4H-1,2,4-三唑-4-基)-苯甲酸的合成

邻氮基苯甲酸;缩合反应;卤代-2-(3-甲基-5-取代-4H-1;2;4-三唑-4-基)-苯甲酸的合成     

1,5-二-(3-硝基苯基)-1,4-戊二烯-3-酮的超声合成

1;5-二-(3-硝基苯基)-1;4-戊二烯-3-酮的超声合成;二-（硝基苯基）-戊二烯-酮;合成;超声;催化     

2-氨基-6-氟-9-(4-羟基-3-羟甲基丁基)嘌呤的合成

报道了2-氨基-6-氟-9-(4-羟基-3-羟甲基丁基)嘌呤(1)的合成, 通过对起始原料2-氨基-6-氯-9-(4-乙酰氧基-3-乙酰氧甲基丁基)嘌呤(2)水解脱去乙酰基, 得到2-氨基-6-氯-9-(4-羟基-3-羟甲基丁基)嘌呤(3). 化合物3与三甲胺乙醇溶液在混合溶剂[V(THF)∶V(DMF)＝3∶1]中反应得到相应的氯化铵盐4, 然后与KF在DMF溶剂中反应, 得到化合物1. 产品经UV-vis, IR, ¹H NMR, ¹⁹F NMR和MS表征. 考察了反应温度、氟化试剂等因素对氟化反应的影响, 为6位含氟的嘌呤核苷类化合物的合成提供了一种直接、简易的新方法.     

6-亚甲基-17α-乙酰氧基-18-甲基-19-失碳-孕甾-4-烯-3,20-二酮的合成新方法研究

报道了16-亚甲基-17α-乙酰氧基-18-甲基-19-失碳-孕甾-4-烯-3,20-二酮的新合成方法. 以左旋18-甲基炔诺酮为原料, 通过脱水、氧化、环合、热解、环氧化、开环氧环、水解七步反应合成了目标化合物, 总收率20.0%. 其中化合物12, 13, 14, 15, 16尚未见文献报道.     

微波作用下1-苯基-5-[5-(芳胺羰基甲硫基)-4-苯基-1,2,4-三唑-3-甲硫基]四唑的合成及生物活性

采用微波和相转移催化法通过1-苯基-5-(4-苯基-1,2,4-三唑-5-巯基-3-甲硫基)四唑(2)与2-氯乙酰芳胺(3)反应高效、快速地合成了10种尚未见文献报道的1-苯基-5-[5-(芳胺羰基甲硫基)-4-苯基-1,2,4-三唑-3-甲硫基]四唑. 其结构经 IR, ¹H NMR, ¹³C NMR 和元素分析表征. 生物活性实验结果表明, 该类化合物在较低浓度下部分化合物对小麦芽有很好的促进作用.     

无催化剂条件下2-氨基-3-氰基-4-芳基-7,7-二甲基-5-氧代-5,6,7,8-四氢-4H-苯并吡喃的合成

芳亚苄基丙二腈;二甲基环己二酮;无催化剂条件下2-氨基-3-氰基-4-芳基-7;7-二甲基-5-氧代-5;6;7;8-四氢-4H-苯并吡喃的合成     

2-氨基-5-(2-氯吡啶-4-基)-1,3,4-噻二唑衍生物的合成及生物活性

酰胺;2-氨基-5-(2-氯吡啶-4-基)-1;3;4-噻二唑衍生物的合成及生物活性     

2-乙氧羰基-3-溴-4-甲基-5-甲酰基-吡咯的合成

2-乙氧羰基-3-溴-4-甲基-5-甲酰基-吡咯的合成;乙氧羰基二甲基吡咯;乙氧羰基溴二甲基吡咯;乙氧羰基溴甲基甲酰基吡咯     

3-巯基-5-芳香基-4-芳基亚甲胺基-4H-1,2,4-三唑的合成及波谱研究

5-取代-4-氨基-3-巯基-1,2,4-三唑与芳香醛在弱酸性乙醇溶液中反应, 合成了一系列3-巯基-5-芳香基-4-芳基亚甲胺基-4H-1,2,4-三唑(3a～3d)及水溶性的3-巯基-5-(D-葡萄糖-1-基)-4-(4-氯代苯基)亚甲胺基-4H-1,2,4-三唑(3e)新化合物. 以元素分析, IR, NMR, MS实验技术对其结构进行了表征, 并研究其NMR波谱特征.     

1-(2, 6, 6-三甲基-1-环己烯基-)-3-甲基-2-丁烯-4-醛合成新工艺

1-(2; 6; 6-三甲基-1-环己烯基-)-3-甲基-2-丁烯-4-醛合成新工艺;(三甲基环己烯基)甲基丁烯醛;卡宾反应; β-紫罗兰酮;三甲基溴化硫     

A Coupling Reaction of 4-Amino-5-mercapto- 3-substituted-1,2,4-triazoles to Generate Symmetrically Substituted Hydrazines

Summary. A novel coupling reaction of 4-amino-5-mercapto-3-substituted-1,2,4-triazoles to generate symmetrically substituted hydrazines, N,N′-bis(5-mercapto-3-substituted-1,2,4-triazol-4-yl)hydrazines was unexpectedly observed. Five examples are presented to demonstrate this reaction. All isolated products were unambiguously characterized.     

1,2,4-Triazoles. Improved synthesis of 5-substituted 4-amino-3-mer-cato-(4H)-1,2,4-triazoles and a facile route to 3,6-disubstituted 1,2,4-triazolo[3,4-b][1,3,4]thiadiazoles

The reaction of thiocarbohydrazide with carboxylic acids at the melting temperature allows an improved preparation of the S-substituted 4-amino-3-mercapto-1,2,4-triazole heterocycles. The crude 4-amino-5-mercapto-1,2,4-triazoles react easily with carboxylic acids or carboxylic acid chlorides to afford the 1,2,4-triazolo[3,4-fc][1,3,4]thiadiazole ring system.     

Chemistry of biureas—I: Cyclisation of ethoxycarbonyl derivatives of thiobiureas and bithioureas

The interaction of ethoxycarbonyl isothiocyanate with semicarbazides or thiosemicarbazides produces 1-ethoxycarbonyl-2-thiobiureas or bithioureas, respectively. The former are cyclisable to 2-ethoxycarbonamido-5-hydroxy-l,3,4-thiadiazole in acid, or to 2(H)-carbamoyl-3-hydroxy-5-alkylthio-1,2,4-triazoles, and thence to 3-hydroxy-5-mercapto-1,2,4-triazole in alkaline media. The ring-closure of the 1-ethoxycarbonylbithioureas proceeds similarly affording, under the influence of acids, 5-amino (or mercapto)-2-ethoxycarbonamido-1,3,4-thiadiazoles. The action of alkali produces compounds derived from 3-hydroxy-5-mercapto-1,2,4-triazole; the isolation, in a selected example, of the 2(H)-phenylthiocarbamoyl-derivative, elucidates the course of this reaction. Hydrazinolysis of 1-ethoxycarbonylbithiourea yields 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole.     

均三唑并噻二唑衍生物的微波合成

在无溶剂无催化剂微波辐射下,羧酸与1,3-二氨基硫脲快速反应高产率得到了3-取代基-4-氨基-5-巯基-1,2,4-三唑,该化合物与苯甲酰氯在无溶剂无催化剂微波促进下可以方便地制备化合物3-取代基-6-苯基-1,2,4-三唑[3,4-b][1,3,4]噻二唑。该方法具有反应时间短、环境友好、易于纯化及高产率的优点。产物结构经IR和1HNMR谱进行了表征。     

SYNTHESIS OF SOME NEW 1,2,4-TRIAZOLO[3,4-b]-THIADIAZOLE DERIVATIVES AS POSSIBLE ANTICANCER AGENTS

3-Substituted-4-amino-5-mercapto-1,2,4-triazoles are versatile synthons for constructing various biologically active heterocycles. Their cyclization with carboxylic acids gives fused five-membered derivatives, whereas with α-bromoketones gives a six-membered heterocycle. In this article we report the synthesis of a series of 1,2,4-triazolo[3,4-b]thiadiazoles 5 starting from 4-amino-3-substituted-5-mercapto-1,2,4-triazoles 3 and fluorobenzoic acids 4 using phosphorous oxychloride as cyclizing agent. Fourteen of the newly synthesized compounds were screened for anticancer properties. Four among them showed in vitro anticancer activity.     

含脱羧脱氢松香基的1,2,4-三唑并[3,4-b]-1,3,4-噻二唑衍生物的合成、表征及抑菌活性

用POCl3为催化剂和脱水剂,3-取代-4-氨基-5-巯基-1,2,4-三唑4和10分别与脱氢松香酸1反应制得14种未见文献报道的3-取代-6-(4′-脱羧脱氢松香基)-1,2,4-三唑并[3,4-b-]-1,3,4-噻二唑衍生物]5a~5e和11a~11i;所有化合物的结构均经IR、¹H NMR、¹³C NMR 和MS测试技术分析确认。 抑菌活性测试表明,目标化合物对白色念珠菌(C.Albicans)、大肠杆菌(E.Coli)、藤黄微球菌(M.Luteus)和痢疾志贺杆菌(S.Dysenteriae)均有一定的抑制作用。     

Studies on Condensed Heterocyclic Compounds XVII. Synthesis of 6-(1-Aryl-5-methyl-1,2,3-triazol-4-yl)-3-phenyl-s-triazolo[3,4-b]-1,3,4-thiadiazoles

Treatment of 4-amino-5-mercapto-3-phenyl-1,2,4-triazole 2 with 1-aryl-4-carboxy-5-methyl-1,2,3-triazoles 1a-1j in a one-step reaction yielded several 6-(1-aryl-5-methyl-1,2,3-triazol-4-yl)-3-phenyl-s-triazolo[3,4-b]-1,3,4-thiadiazoles 3a-3j . The structures of all the products were established on the basis of elemental analyses and spectral data. The fragmentation of the mass spectra of 3a-3j under electron impact was discussed.     

NOVEL SYNTHESIS OF CONDENSED HETEROCYCLIC SYSTEMS CONTAINING 1,2,4-TRIAZOLE RING

3-Aryl-6,7-dihydro-s-triazolo[3,4-b][1,3]thiazines and 3-aryl-5,6-dihydro-thiazolo[2,3-c]-s-triazoles were synthesized by nucleophilic substitution of 3-aryl-5-mercapto-1,2,4-triazoles with 1,3-dibromopropane and 1,2-dichloroethane. And the bis-Mannich reaction of 3-aryl-5-mercapto-1,2,4-triazoles with formaldehyde has been studied.     

含双-三唑并噻二唑环的庚烷类衍生物的合成及抗菌活性

The aroylhydrazides were prepared by esterification and hydrazinolysis of corresponding aromatic carboxylic acids.The reaction of aroylhydrazides with CS2/KOH in absolute ethanol gave potassium aroyldithiocarbazates and then hydrazinolysis of potassium aroyldithiocarbazates with hydrazine hydrate afforded 3-aryl-4-amino-5-mercapto-1,2,4-triazoles(1a～1g).New seven compounds of bis[(3-aryl)-s-triazolo[3,4-b]-[1,3,4]thiadiazole derivatives(2a～2g) were synthesized in high yields by cyclization of nonanedioic ac...