2-(4-溴苯基)-3,3-二苯基丙烯腈的合成及光物理性质

以甲苯为溶剂，利用二苯甲酮与对溴苯乙腈在碱性条件下经Knoevenagel缩合反应，合成了2-(4-溴苯基)-3,3-二苯基丙烯腈（Br-TPAN），其结构和性能经FL, UV-Vis, ¹H NMR, ¹³C NMR, HR-MS(ESI), XRD和TGA表征。并研究了反应温度和反应时间对Br-TPAN收率的影响。结果表明：于80 ℃反应10 h, Br-TPAN收率大于80%。 Br-TPAN具有结晶诱导发光特性。     

新型双-1,4-二氢吡啶的水相微波辅助合成

采用微波辅助合成法,以四叔丁基溴化铵（TBAB）为催化剂,水为溶剂,3,3-二乙氧基丙酸乙酯,胺和二醛（或醛和二胺）为原料,经Hantzsch反应合成了11个双-1,4-二氢吡啶化合物(I-1~I-7和II-1~II-4),其中I-3~I-7和II-2~II-4为新化合物,其结构经¹H NMR, ¹³C NMR和HR-MS(ESI)表征。以I-1的合成为例,考察了相转移催化剂、微波功率、反应温度和反应时间对产率的影响。在最佳条件［TBAB 2.5 mol%,于100 W, 60 ℃微波反应30 min］下,I和II产率分别为70.9%~92.5%和79.8%~95.5%。     

新型3-吗啉-3-四取代氧化吲哚的合成

以3-卤氧化吲哚和吗啉（或硫代吗啉）为起始原料，碳酸钠为催化剂，于60 ℃发生3-叔胺基化反应，合成了10个新型的3-吗啉四取代氧化吲哚 (3aa~3bh)，收率86%~94%，其结构经¹H NMR, ¹³C NMR和HR-MS（ESI-TOF）表征。     

微波辅助合成N-（2-嘧啶基）吲哚化合物

以取代吲哚和2-氯嘧啶为原料,通过微波辅助合成N-（2-嘧啶基）吲哚化合物,对碱、溶剂、反应温度、反应时间、微波功率等进行了优化,筛选得到的最佳反应条件为：以碳酸铯为碱,DMSO为溶剂,于微波功率500 W、145℃下反应5min。在最佳反应条件下,3个4-位取代吲哚化合物均可与2-氯嘧啶反应,收率大于80%,产物结构经¹H NMR和¹³C NMR确证。      

(S)-(4-溴-2-甲苯)(3-甲基吗啉)甲酮的合成

以(S)-2-氨基丙醇和氯乙酰氯为起始原料,经酰化和环合反应制得(S)-5-甲基吗啉-3-酮（4）; 4经还原制得(S)-3-甲基吗啉(5); 5与4-溴-2-甲基苯甲酸酰化缩合合成了(S)-(4-溴2-甲基苯基)(3-甲基吗啉)-甲酮,总收率57%,其结构经¹H NMR 和 ¹³C NMR确证。     

1,3-二芳基-1丙酮类化合物的合成

以取代苯乙酮和取代芳香醛为原料,制得一系列1,3-二芳基-1-氧代丙烯类化合物(1a~1j); 1a~1j和对甲苯磺酰肼(2)经还原反应合成了10个1,3-二苯基-1-丙酮类化合物(3a~3j, 3h为新化合物),其结构经¹H NMR, ¹³C NMR, IR和HR-MS（ESI）确证。研究了碱、溶剂、温度和投料比γ[n(1a)/n(2)/n(碱)]对3a产率的影响。结果表明：γ=1/2/2,磷酸钾为碱,乙醇为溶剂,于80 ℃反应4 h, 3a产率最高（80%）。     

4-(3-氯苯乙基)呱啶的简便合成

以廉价易得的N-Boc呱啶-4-甲醇（1）和间氯苄氯（3）为原料,经Swern 氧化、Wittig反应、钯碳催化加氢和脱保护基反应合成目标化合物4-(3-氯苯乙基)呱啶盐酸盐(7)。路线总收率达到56%,化学纯度96.6%。加氢不脱氯反应的最佳反应条件为：以含量为10%干钯碳催化加氢,二氧六环为溶剂,反应时间3h。化合物7的结构及纯度经¹H NMR,¹³C NMR和MS（EI）确证。该合成方法具有反应条件温和、操作简单、收率高等优点。      

O-炔丙基-N,N-二(2-氯乙基)-4-氨基苯酚的合成

以对氨基苯酚（1）为原料,经氨基的羟乙基化、酚羟基的苄基保护、氯代、脱保护制得N,N-二 (2-氯乙基) -对氨基苯酚（5）;在碳酸铯作用下,5与溴丙炔经O-烷基化反应合成了新化合物--O-炔丙基-N, N-二(2-氯乙基)-4-氨基苯酚,其结构经¹H NMR, ¹³C NMR和MS表征。     

一锅法合成2-苄基-2,3-丁二烯腈类化合物

氮气保护下，以（三苯基膦）乙腈、苄基溴、乙酰氯为原料，三乙胺为碱，在二氯甲烷中经一锅法反应合成了12个2-苄基-2,3-丁二烯腈类化合物（3a~3l），其中3b~3l为新化合物，其结构经¹H NMR，¹³C NMR和HR-MS(ESI)表征。     

1-(4-叔丁基苯基)-1,1-二[4-(4-硝基苯氧基)\]苯基乙烷的合成及其溶解性研究

以叔丁基苯为起始原料,经3步反应制得了一种新化合物1-(4-叔丁基苯基)-1,1-二[4-(4-硝基苯氧基)]苯基乙烷（3）,总收率61.14%,其结构经¹H NMR和IR表征。3可溶于非极性溶剂（石油醚除外）和极性非质子溶剂。     

1-羟基苯并三唑的合成工艺研究

研究了以邻硝基氯苯和水合肼为原料 ,在微正压下采用蒸馏分水工艺合成 1 羟基苯并三唑的工艺过程。讨论了溶剂、原料摩尔比、反应进间、反应温度等因素对反应的影响 ,最适宜操作条件为 :邻硝基氯苯与水合肼的摩尔比为 1∶4、溶剂正庚醇用量是邻硝基氯苯质量的 90 %、反应温度 1 1 8℃、反应时间 5h ,产品收率达 98.7%。     

Synthesis of Pyrimidines,Thienopyrimidines, and Pyrazolopyrimidines

5-Ethoxycarbonyl-4-methyl-2-phenylpyrimidin-6(1H)-thione ( 3 ), which was prepared from the reaction of ethyl g -aminocrotonate 1 with benzoyl isothiocyanate ( 2 ) in refluxing acetone, was reacted with a series of halopgenated reagents to give S-alkyl derivatives 4a-g . Upon treatment of compounds 4a-c with sodium ethoxide were cyclized into thienopyrimidine 10a-c . Pyrimidinethione 3 was reacted with hydrazine hydrate to give hydroxypyrazolopyrimidine derivative 6 . The later compound was obtained by heating compound 4a with hydrazine hydrate under neat conditions, but when the reaction was carried using hydrazine hydrate in ethanol, the corresponding carbohydrazide 5 was produced.     

新型席夫碱基杯[4]冠醚衍生物的合成

杯[4]-1,3-二酯衍生物与水合肼反应后再与二水杨醛二甘醚发生"1 1"分子间缩合,高产率合成了新型席夫碱基杯[4]冠醚衍生物,其结构经1HNMR,IR,MS和元素分析表征。     

Synthesis,Crystal Structure and Bioactivity of Phenazine-1-carboxylic Acylhydrazone Derivatives

A phenazine-1-carboxylic acid intermediate was synthesized from the reaction of aniline and 2-bromo-3-nitro-benzoic acid. It was then esterified and reacted with hydrazine hydrate to afford phenazine-1-carboxylic hydrazine. Finally, 10 new hydrazone compounds 3a–3j were obtained by the condensation reaction of phenazine-1-carboxylic acid hydrazide and the respective aldehyde-containing compound. The structures were characterized by ¹H and ¹³C NMR spectroscopy, MS and single crystal X-ray diffraction. The antitumor activity of the target compounds in vitro (HeLa and A549) was determined by thiazolyl blue tetrazolium bromide. The results showed that compound (E)-N′-(2-hydroxy-4-(2-(piperidine-1-yl) ethoxy) benzyl) phenazine-1-carbonyl hydrazide 3d exhibited good cytotoxic activity.     

1-芳基亚甲基-2-(6-(3,5-二甲基-1H-吡唑-1-基)-1,2,4,5-四嗪-3-基)肼的合成及抗菌活性

以水合肼和硝酸胍为原料,经过环合、氧化和肼化,得到3-(3,5-二甲基-1H-吡唑-1-基)-6-肼基-1,2,4,5-四嗪(4),以此为原料和不同芳香醛发生腙化反应,得到系列1-芳基亚甲基-2-(6-(3,5-二甲基-1H-吡唑-1-基)-1,2,4,5-四嗪-3-基)肼(5),产物经元素分析、1H NMR、IR和MS表征。所合成的系列化合物抗菌活性测试表明,它们对大肠杆菌、金黄色葡萄球菌、枯草杆菌等3种细菌表现出一定程度的抑制活性。     

Synthesis,Antioxidant, Antituomer Activities of Some New Thiazolopyrimidines,Pyrrolothiazolopyrimidines and Triazolopyrrolothiazolopyrimidines Derivatives

Reaction of 6‐amino‐2‐thiouracil 1 with ethyl bromoacetate yielded ethyl 2‐(7‐amino‐2,5‐dioxo‐3,5‐dihydro‐2H‐thiazolo[3,2‐a]pyrimidin‐6‐yl)acetate 2 . Reaction of 2 with sodium ethoxide afforded the pyrrolothiazolopyrimidine derivative 3 . Compound 2 reacted with hydrazine hydrate to give 7‐amino‐thiazolopyrimidine‐carbohydrazide 4 . The latter compound 4 reacted with carbon disulphide to form 7‐amino‐6‐(oxadiazolylmethyl) thiazolopyrimidine 5 . Compound 5 was heated in methanol to yield 9‐thioxotriazolopyrrolothiazolopyrimidine 6 . Also, the reaction of 3 with aromatic aldehydes afforded the diarylmethylenepyrrolothiazolopyrimidine derivatives 7a‐c . The latter compounds 7a‐c underwent cyclocondensation with hydroxylamine to give diaryldioxazolopyrrolothiazolopyrimidine derivatives 8a‐c . The new prepared compounds were subjected for antioxidant and antituomer studies, some of these compounds exhibited promising activity.     

苄连氮桥联双硫杂杯[4]芳烃的合成

硫杂杯[4]二醛基衍生物(1)在水合肼中肼解,合成了新化合物硫杂杯[4]二醛腙基衍生物(2);1和2在弱酸的催化下反应合成了新的具有对称结构的苄连氮双硫杂杯[4]芳烃(3);2和3的结构经1H NMR,IR,ESI-MS和元素分析表征.     

一种以三聚氯氰为桥基的新型小分子功能活性染料的合成

以对氨基苯甲酸甲酯和水合肼为原料,经酰胺化反应制得对氨基苯甲酸甲酰胺,进一步与水杨醛通过还原氨化反应生成席夫(1）;以罗丹明B和水合肼为原料,1经闭环反应制得罗丹明B酰肼（2）; 2在四氢呋喃溶剂中与三聚氯氰经缩合取代反应生成一缩产物（3）; 3进一步在四氢呋喃中与1于45~50 ℃回流6 h,经取代反应生成二缩产物,其结构经¹H NMR, MS, IR和元素分析表征。     

Synthesis of heierocyclic compounds from 2-phenyl-1, 2,3-triazole-4-formylhydrazine

2-Phenyl-1, 2, 3-triazole-4-formylhydrazine (2) was prepared by hydrazinolysis of the corresponding ester 1. Reaction of 2 with CS2/KOH gave the oxadiazole derivatives (3) which via, Mannich reaction with different dialkyl amines furnished 3-N, N-dialkyl derivatives (4a-c). Also, condensation of 2 with appropriate aromatic acid in POCl3 yielded oxadiazole derivatives (5a-c), or with aldehydes and ketones afforded hydrazones (6a-c). Cyclization of (6a-c) with acetic anhydride gave the desired dihydroxadiazole derivatives (7a-c). On the other hand, reaction of dithiocarbazate (8) with hydrazine hydrate gave the corresponding triazole derivative (9) which on treatment with carboxylic acids in refluxing POCl3 yielded s-triazole[3,4-b]-1, 3, 4-thiadiazole derivatives (10a-b). The structures of all the above compounds were confirmed by means of IR, 1H NMR, MS and elemental analysis.     

Utility of 4‐Benzylidene‐2‐phenyl‐5(4H)‐oxazolone in Synthesis of Triazine,Oxadiazole and Imidazole Derivatives of Anticipated Biological Activity

Treatment of oxazolone 1 with hydrazine hydrate at room temperature gave the (Z)‐configurated isomer hydrazide (Z)‐ 3 (high yield). However, refluxing 1 with hydrazine hydrate yielded the (E)‐configurated isomer hydrazide (E)‐ 2 (low yield).The hydrazide derivative (Z)‐ 3 has been utilized as synthon for the synthesis of 1,2,4‐triazinone, imidazolone, and oxadiazole derivatives through appropriate routes. The thiosemicarbazide and semicarbazide derivatives are synthesized by different routes. The structures of the new compounds were established on the basis of IR, ¹H‐NMR, mass spectral data, and elemental analysis.