A convenient synthesis of 2-aryl substituted benzo[f] [1,2,4]triazolo[1,5-a]azepine derivatives

A convenient synthetic pathway to 2-aryl-5,6-dihydro-4H-benzo[f][1,2,4]triazolo[1,5-α]azepine derivatives 7 was developed. The synthesis was based on the cycloaddition of the 1,2,3,4-tetrahydronaphthalene a-acetoxy azo compounds 3 with Ar-CN in the presence of AlCl3 and the consecutive ring enlargement.     

Synthesis of N-（α-Alkoxyalkyl）benzotriazoles Catalyzed by Acidic Ionic Liquid at Room Temperature

N-（α-Alkoxyalkyl）benzotriazoles were synthesized via the condensation of benzotriazole with various aldehydes and alcohols catalyzed by acidic ionic liquid [hmim]HSO4 at room temperature. The yield was up to 99%. This novel method was effective when triethoxymethane was utilized instead of alcohols. Moreover, acidic ionic liquid could be reused easily with no significant degradation of its catalytic activity.     

Preparation ,Structural Characterization and Luminescent Property of Binucleasr Silver（Ⅰ）Complex Formed by Benzotriazole and 1—Hydroxymethyl Benzotriazole

Dinuclear silver (I) six‐membered ring complex [Ag₂ (bta)₂ ‐(hmbta)₂] (ClO₄)₂ (3) has been synthesized by the reaction of benzotriazole (bta) (1) and 1‐hydroxymethyl benzotriazole (hmbta) (2) with Ag (CH₃CN)₄ClO₄. The structures of compound 2 and Complex 3 have been studied by single crystal X‐ray diffraction analysis. The change of luminescent intensity of 1, 2 and 3 was reported. Compound 2 crystallizes in the monoclinic system with space group P2 (1)/c, a = 0.7655 (10) nm, b = 1.0126 (14) nm, c =0.9502 (13) nm, β = 95.07 (2)°, V = 0.7337 (17) nm³ and Z = 4. Complex 3 crystallizes in the triclinic system with space group P1, a = 0.73611 (18) nm, b = 0.9152 (2) nm, c = 1.2277 (3) nm, β = 87.170 (5)°, V = 0.8221 (3) nm³ and Z = 1. The main structural feature of complex 3 is a symmetric dinuclear six‐membered ring formed by two silver (I) atoms and four N‐atoms from two benzotriazoles. The second structural feature of complex 3 is the τ‐τ stacking interaction between two adjacent molecular planes, which forms the two‐dimentional layer structure. Besides, compared with 2, the luminescent intensity of complex 3 shows a remarkable enhancement.     

Triazole and Benzotriazole Derivatives as Novel Inhibitors for p90 Ribosomal S6 Protein Kinase 2： Synthesis, Molecular Docking and SAR Analysis

A series of triazole and benzotriazole derivatives as novel p90 ribosomal S6 protein kinase 2 （RSK2） inhibitors were designed and synthesized. The in vitro activities against RSK2 were evaluated, and among 14 compounds, compounds 5, 6, 11, 12, 13 and 14 exhibited enzyme IC50 values of 8.91, 2.86, 3.19, 3.05, 4.49 and 2.09 μmol/L re- spectively. The proposed binding modes were simulated using molecular docking method, and the docking results coupled with the stmcture-activi1：y relationship （SAR） analysis indicated that all these active compounds bound to the RSK2 ATP binding site at NTKD, and the electron-donating groups on the 4-position of phenyl were the deter- minant point for the inhibitory activity.     

固相萃取高效液相色谱-串联质谱法测定地表水中苯并三唑类及苯并噻唑类衍生物

建立了环境水样中8种苯并三唑类和苯并噻唑类化合物:苯并三唑(1H-benzotriazole,BTri)、5-甲基苯并三唑(5-Methyl-1H-benzotriazole,5-TTri)、5,6-二甲基苯并三唑(5,6-Dimethyl-1H-benzotriazole,5,6-DMBTri)、5-氯-苯并三唑(5-Chloro-1H-benzotriazole,5-ClBTri)、1-羟基苯并三唑(1-Hydroxybenzotriazole,1-OHBTri)、苯并噻唑(Benzothiazole,BT)、2-氨基苯并噻唑(2-Aminobenzothiazole,2-ABT)和2-甲基苯并噻唑(2-Methylbenzothiazole,2-TBT)的高效液相色谱-串联质谱(LC-MS/MS)分析方法。200 mL环境水样经0.22μm滤膜过滤后用盐酸(1∶1)调至pH 3.0,过HLB固相萃取柱,经3 mL 10%甲醇水溶液淋洗,6 mL丙酮-甲醇(2∶8,体积比)洗脱。目标化合物经Hypersil GOLD型色谱柱(150 mm×2.1 mm)结合甲醇-水-乙腈梯度洗脱分离后,用正离子多重反应监测模式进行质谱分析。结果表明,1-OHBTri、BT及2-TBT的线性范围为8~1 000μg/L,其他5种化合物的线性范围为1.6~1 000μg/L,相关系数均大于0.99。8种化合物的基质加标回收率为59.8%~98.7%,相对标准偏差(n=5)为0.9%~12.5%,方法的检出限(S/N=3)为0.03~1.4μg/L。     

5-甲基苯并三唑-1-乙酸铕三元配合物的合成及表征

以5-甲基-苯并三唑-1-乙酸和1,10-邻菲啰啉为配体,采用溶液法合成了一种铕配合物。通过元素分析、配位滴定、摩尔电导率、红外光谱和紫外光谱对其进行表征。其组成可能为Eu(L)3phen·3.5H2O(HL=5-甲基-苯并三唑-1-乙酸,5-mbtaa;phen=1,10-邻菲啰啉)。使用热分析和荧光光谱研究了配合物的性质。热分析结果显示:铕配合物具有较好的热稳定性。荧光光谱显示:该配合物发出Eu(Ⅲ)特征荧光,并且5-甲基-苯并三唑-1-乙酸是较好的敏化剂。     

2-十二烷基二硫代-4-苯基-1,3,4-噻二唑-5-硫酮的合成及其对铜的缓蚀性能

合成了2-十二烷基二硫代-4-苯基-1,3,4-噻二唑-5-硫酮(DPTT),用元素分析、IR1、H NMR等技术对化合物进行了结构表征.采用动态旋转挂片法考察了DPTT和苯并三唑(BTA)复配时对铜的缓蚀作用.结果表明,单一DPTT在浓度为3.0 mg/L时缓蚀效果最佳;DPTT与BTA复配使用时显示出较好的协同效应,1.0 mg/L DPTT和1.0 mg/L BTA复配时缓蚀效果最好.     

Synthesis and Crystal Structure of 1-[4-(Pyrimidin-2-yl)piperazin-1-ylmethyl]-1H-benzotriazole

1 INTRODUCTION Based on the reported 1.65 ? high resolution crystal structure of spinach KARI (ketol-acid reduc- toisomerase) complex[1], we obtained 279 molecules with low binding energy toward KARI from MDL/ ACD 3D database searching, using program DOCK 4.0[2]. These potential structures provide further information for the design of new KARI inhibitors, one of novel derivatives of which as the title com- pound has been synthesized. Its crystal structure will provide us more inf…     

3类高关注紫外线吸收剂的前处理与检测技术研究进展

紫外线吸收剂是一种具有强烈吸收紫外线作用的光稳定剂,会对生态环境以及人体健康造成危害,国内外许多国家已制定相关法规限制其使用。该文综述了近几年来国内外关于二苯甲酮类、三嗪类和苯并三唑类3类紫外线吸收剂检测的研究现状,分别对样品前处理与检测技术进行了详细介绍,并对其研究发展趋势进行了展望。