1,2-二乙酰氧甲基碳硼烷的合成

以6,9-二乙腈十硼烷和1,4-二乙酰氧基-2-丁炔为原料,合成了高纯度的1,2-二乙酰氧甲基碳硼烷,产率81.2%,纯度96.2%,其结构经UV-Vis,<'1>H NMR,<'11>B N-MR,IR和元素分析表征.     

5(6)-羧基荧光素标记2′-脱氧尿苷的合成

以5-碘-2'-脱氧尿嘧啶为起始原料, 5(6)-羧基荧光素为荧光标记物, 经6步反应合成了5(6)-羧基荧光素标记的2′-脱氧尿苷, 并利用高效液相色谱(HPLC), ¹H NMR和¹³C NMR对目标化合物的纯度和结构进行了表征.     

4-甲基-苯磺酸-2-氧-2-[3-(5-芳基-[1,3,4]噁二唑-2-基)-硫脲]-乙基酯的合成及生物活性研究

合成了12个未见文献报道的4-甲基-苯磺酸2-氧-2-[3-(5-芳基-[1,3,4]噁二唑-2-基)-硫脲]-乙基酯, 其结构经元素分析、¹H NMR和IR确证. 初步活性测试结果表明: 部分化合物有较好的杀菌活性.     

二{2-{2-{9-乙基-6-[2-(8-羟基喹啉-2-基)乙烯基]咔唑-3-基}乙烯}-8-羟基喹啉}锌配合物的合成与荧光光谱特性

合成了新的N-乙基咔唑衍生物: 3,6-二[2-(8-羟基喹啉基)乙烯基]咔唑(4)及其锌配合物(5); 化合物4经质谱、红外光谱、核磁共振氢谱、元素分析表征其结构, 并测定了它的荧光光谱. 结果显示: 化合物4的荧光发射为蓝绿色光(500 nm), 其发射光谱随着溶剂极性的增大荧光光谱向长波方向移动(即发生红移); 同时, 考察了化合物5的荧光性质, 其荧光发光峰值为600 nm, 与2-甲基-8-羟基喹啉锌相比, 发生了明显的红移.     

3-吗啉基氟化硼络合二吡咯甲川类化合物的合成及反应机理研究

以对羟基苯甲醛和吡咯为原料,合成了3-吗啉-8-[4'-(3-吗啉丙氧基)苯基]氟化硼络合二吡咯甲川和3-吗啉-8-(4'-甲氧基苯基)氟化硼络合二吡咯甲川,其结构经过1H NMR和LC-MS分析表征,通过相似性试验和晶体的培养对吗啉直接取代氟化硼络合二吡咯甲川(BODIPY)类化合物3-H的反应机理进行研究.     

含嘧啶基团的新型亲水性共轭大环化合物的合成

以三乙甘醇单甲醚为原料,制得化合物1和2; 1和2经取代反应制得1-【2-{1-[2-(2-甲氧基乙氧基)乙氧基]乙氧基}甲基-3-[2-(2-甲氧基乙氧基)乙氧基]乙氧基】丙氧基-3,5-二溴苯(3)和1-[2-(2-甲氧基乙氧基)乙氧基]乙氧基-3,5-二溴苯(4); 3和4分别与双频那醇合二硼反应制得化合物5和6; 6与5-溴-2-碘嘧啶发生Suzuki-Miyaura交叉偶联反应制得化合物7; 5与7在铂催化下发生Suzuki-Miyaura交叉偶联反应合成了一个新型的共轭大环化合物,其结构经¹H NMR, ¹³C NMR和MALDI-TOF-MS表征。     

一步法合成N-1,3-二羟基丙烷-2-基烷基乙酰胺

以5-氨基烷基-2,2-二甲基-1,3-二噁烷为起始原料, 乙酸酐为酰化剂, 一步法选择性地合成氨基二醇类氨基乙酰化产物N-1,3-二羟基丙烷-2-基烷基乙酰胺. 该方法操作简便, 收率高. 所合成的4个新化合物的结构均经FTIR, ¹H NMR, ¹³C NMR及HRMS确证. N-3-(1,3-二羟基丙烷-2-基)丙基乙酰胺(1a)作为关键的中间体, 可以用于HIV-1 Tat/ PCAF BRD抑制剂4的合成.     

新型两亲性氮杂六芳基苯的合成

以5-溴-2-十二烷基嘧啶为原料,经Sonogashira偶联等反应制得1,2-双(2-十二烷基嘧啶-5-基)乙炔(4); 1-溴-4-(2-(2-(2-甲氧基乙氧基)乙氧基)乙氧基)苯(5)与双频哪醇合二硼反应制得化合物(6); 4,4′-二溴苯偶酰与1,3-二苯基丙酮经羟醛缩合反应制得四芳基环戊二烯酮衍生物(7); 化合物4与7经Diels-Alder反应制得化合物8; 8与6〖STBZ〗通过Suzuki-Miyaura偶联反应合成新型两亲性氮杂六芳基苯(9),化合物6~9为新化合物,其结构经¹H NMR, ¹³C NMR和HR-MS(MALDI-TOF)表征。     

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.     

新型4,4′-二对吡唑苯乙烯基-2,2′-联吡啶的合成及其光学性质

以吡唑苯甲醛和4-甲基吡啶为原料,经缩合反应合成了一种新型的联吡啶衍生物-一4,4′-二对吡唑苯乙烯基_2,2′-联吡啶(1),其结构经<'1>H NMR,IR和MS表征.用UV和单光子荧光光谱研究了1的线性光学性质.     

Anomalous fluorescent responses of 9-fluorenecarboxamide derivatives possessing benzo-15-crown-5.

A new fluorescent ionophore for alkaline earth metal ions, 4'-(9-fluorenecarboxamido)benzo-15-crown-5 (3), was synthesized; its photochemical behavior was investigated using UV, fluorescence, (1)H NMR, and (13)C NMR spectrometry. In the absence of a metal ion, the fluorene moiety showed weak fluorescence emission (fluorescence "Off" state). However, complexation with metal ions greatly enhanced the fluorescence intensity (fluorescence "On" state).     

2-氨基-5-(对二甲氨基)苯基-1,3,4-噻二唑:Hg2+的选择性荧光传感分子

设计合成了结构简单的分子内电荷转移荧光传感分子1,3,4-噻二唑类衍生物(1), 实现了水-乙醇(体积比1∶9)混合溶剂中Hg2+的荧光猝灭型选择性灵敏传感, 荧光猝灭常数达5.5×105 mol-1·L, Hg2+线性响应范围为5.0×10-6～5.0×10-5mol/L. 基于等摩尔连续变化法、红外光谱和核磁滴定实验结果提出了传感分子1与Hg2+的1∶1型结合模式, 其中1-位S原子和2-位胺N原子为Hg2+配位原子; 结合光谱变化讨论了Hg2+结合显著增强分子内电荷转移的荧光猝灭机理.     

含二茂铁基荧光探针对H2S的识别

以乙酰二茂铁和蒽醛为原料,合成了一种新的反应型荧光探针1-二茂铁基-3-(9-蒽基)丙烯酮,经1H NM R,13C NM R,IR,LC-M S等手段表征确证。基于Michael加成引起的电子转移机制,利用硫化氢的强亲核性,以荧光滴定法考察了该化合物在生理条件下对硫化氢的识别作用,得出其最佳识别时间为50 min,最佳识别浓度为50μmol/L,且多数离子不会对其识别作用产生干扰。这种能稳定检测的,具有高选择性、高灵敏度的反应型荧光探针化合物,可用于生物医药领域。     

GFP生色团衍生物的合成及其荧光性能

以N-甲基乙酰胺或N-甲基苯甲酰胺为起始原料,与氯乙酰氯经酰化反应后,与叠氮钠经取代反应制得二酰亚胺(2); 2在三苯基膦的催化下发生分子内氮杂Witting反应制得关键中间体--咪唑啉酮(3); 3与芳醛在碱性条件下经缩合反应合成了8个新型的GFP生色团衍生物(5a~5h),其结构经¹H NMR和¹³C NMR表征。对5a~5h的激发波长和发射波长进行了研究。结果表明,与对羟基苯咪唑啉酮(p-HOBDI)相比,大部分化合物的发射波长发生了比较显著的红移,其中2-羟基5-硝基苯咪唑啉酮(5f)的发射波长达614 nm。     

新型香豆素类荧光探针的合成及其对Cu~(2+)的识别性能

以2-羟基-4-甲氧基苯甲醛和丙二酸二乙酯为起始原料,设计并合成了一种新型的Cu~(2+)荧光探针7-甲氧基-2-氧代-N-[2-(苯基氨基)乙基]-2H-色烯-3-甲酰胺(NPC),其结构经~1H NMR,~(13)C NMR,MS(EI)和元素分析表征。并研究了室温下,NPC在乙醇和水的混合溶液中对Cu~(2+)的识别性能。结果表明:NPC对Cu~(2+)表现出荧光猝灭效应,具有对Cu~(2+)的选择性识别性能。     

过氧化物酶新型荧光底物3,4-二氢-2(1H)-喹喔啉酮的反应机理及性能的研究

合成了过氧化物酶新型荧光底物3,4-二氢-2(1H)-喹喔啉酮(DHQXL). 在过氧化物酶催化下,该化合物可被H₂O₂氧化生成强荧光物质2(1H)－喹喔啉酮(QXL). 用高压液相色谱法分离得荧光产物纯品,经核磁共振谱和质谱证实其结构,确证了提出的酶催化反应机理. 对该化合物作为荧光底物的性能研究表明,它是一个很有应用前景的过氧化物酶的新型荧光底物.     

含有电子传输基团的双齿配体及铕配合物Eu(DBM)3(DPOP)的制备与发光性能的研究

1, 3, 4-oxadiazole-contanining ligand DPOP(DPOP=2-(11-dipyrido[3, 2-a: 2′, 3′-c]phenazine)-5-p-tolyl-1, 3, 4-oxadiazole) was synthesized by a convenient method and characterized by elemental analysis, IR, ¹H NMR. Then, corresponding Eu(Ⅲ) complex [Eu(DBM)₃(DPOP)] (DBM=1, 3-diphenyl-1, 3-propanedionate) was prepared and characterized by elemental analysis, IR. The photophysical properties of ligand and its europium complex were investigated. The ligand emitted at 443 nm. There were different PL spectra in solid state and in solution of Eu(DBM)₃(DPOP). There are two fluorescent peaks at 614 nm, 400 nm in dichloromethane solution of Eu(DBM)₃(DPOP), but in solid state only red emission was observed. This result indicated that efficient energy tranfer could take place from DPOP ligand to europium ion in Eu-complex solid.     

聚(2-甲氧基-5-丁氧基)对苯乙炔的合成、表征及光性能研究

１９９０年,Ｂｕｒｏｕｇｈｅｓ等［１］发现聚对苯乙炔（ＰＰＶ）类衍生物不仅是导电高分子材料,而且也是性能优良的发光材料．随后,许多科学家立即将注意力集中于这类共轭聚合物的合成及光性能的研究上,并取得了可喜的研究成果［２］．目前,对ＰＰＶ衍生物的合成,...     

A dual-function chemosensor based on coumarin for fluorescent turn-on recognition of Hg2+ and colorimetric detection of Cu2+ in aqueous media

A novel coumarin derivative CTT was synthesized via the condensation of 7-(N,N-diethylamino) coumarin-3-aldehyde with 5-amino-1,3,4-thiadiazole-2-thiol and its structure was characterized using infrared spectroscopy (IR), ¹H NMR, mass spectrometry (MS) techniques, and elemental analysis. The recognition properties of CTT with metal ions were investigated in CH₃CN–H₂O (v/v = 1/1) solution using UV–vis absorption and fluorescence emission spectrum method. The results showed that CTT could monitor Cu²⁺ and Hg²⁺ simultaneously as a dual-function chemosensor in CH₃CN–H₂O (v/v = 1/1). CTT could be used to detect Cu²⁺ colorimetrically; when using CTT, a color change from yellowish-brown to yellowish-green could be readily observed by the naked eye. CTT showed turn-on fluorescent recognition of Hg²⁺, the fluorescence enhancement was attributed to the inhibited C=N isomerization and the obstructed excited state intramolecular proton transfer (ESIPT) of CTT. The recognition mechanism of CTT for Cu²⁺ and Hg²⁺ was studied by experiments and theoretical calculations, respectively. Therefore, CTT has the ability to be a “single chemosensor for dual targets.”     

A highly sensitive naphthalimide-based fluorescent probe for detection of Cu2+ via selective hydrolysis reaction and its application in practical samples

A novel fluorescent probe CN3, containing 1,8-naphthalimide and picolinate units, was synthesized, and its structure was characterized by ¹H nuclear magnetic resonance spectroscopy (H NMR), ¹³C nuclear magnetic resonance spectroscopy (C NMR), and mass spectroscopy techniques. The detection property of CN3 toward copper ions (Cu²⁺) has been investigated in ethanol–HEPES buffer (v/v = 1/1, pH = 7.40) solution by UV–Vis absorption and fluorescence emission spectra. The results showed that CN3 had a highly selective and sensitive fluorescence quenching response to Cu²⁺, which was attributed to the generation of weak fluorescent N-ethyl-4-hydroxyphenyl-1,8- naphthalimide (compound 2) in polar ethanol–HEPES buffer (v/v = 1/1, pH = 7.40) via selective hydrolysis reaction. The detection of CN3 for Cu²⁺ was not influenced in the presence of other competing metal ions, and the limit of detection was as low as 50.0 nM. Therefore, the color of CN3 changed from colorless to yellowish when the Cu²⁺ was added. Furthermore, the fluorescent probe CN3 was utilized to detect Cu²⁺ in real water samples with fine performance.