1,2-苯并噻嗪类化合物的设计、合成及抗肿瘤活性研究

依据生物电子等排原理,设计合成了13个全新结构的1,2-苯并噻嗪类化合物,其结构均经IR,1H NMR,13C NMR和MS确证.以A431,A549,MDA-MB-468和HL60 4种细胞株为活性筛选对象,采用四甲基偶氮唑盐(MTT)法进行初步的体外抗肿瘤活性研究.结果表明,部分化合物对肿瘤细胞有一定的抑制活性,其中化合物5b对A431具有显著的抑制活性,IC50值为1.57μmol/L,化合物9a对A431,A549和MDA-MB-468 3种细胞株的抑制活性均强于阳性对照药gefitinib.并采用Moe软件对所合成的化合物与表皮生长因子受体(EGFR)结合位点进行对接,以进一步阐释所合成化合物的作用靶标.     

新型喹唑啉类酪氨酸激酶化学抑制剂的设计与合成

以6-氨基藜芦酸和醋酸甲脒为起始原料,合成了一系列4-位具有不同芳胺基团,6,7-位引入不同取代基的新型喹唑啉类酪氨酸激酶化学抑制剂,其结构经1H NMR表征.     

A Facile Synthesis of Various Butenolides

The synthesis of α'-acyloxy-α,β-unsaturated cyclic ketones from the corresponding α,β-unsaturated cyclic ketones by using manganese (III) acetate in combination with 2-chloropropionic acid followed by subsequent Arbuzov and intramolecular Horner-Emmons cyclization reactions provided a convenient synthetic pathway to various butenolides 4a-d.     

A Facile Synthesis of Pyrrolidine Derivatives

The Amaryllidaceae alkaloids have attracted considerable attention for their interesting biological activities. [1] Many of these tyrosine derived alkaloids[2] incorporate a hexahydroindole moiety in the structural skeletons. New approaches towards the synthesis of hexahydroindole core have been a topical interest for the synthetic community.Herein we report an experimentally very simple method for the synthesis of hexahydroindole by aminocylization. Four kinds of N-substituted have been demonstrate to be effective to this cyclization. The results were summarized in Figure 1.     

A Facile Synthesis of Biscyclopropane Derivatives

Abstract: Bis(dibutyltelluronium)p-xylylene dibromide reacts easily with α,β-unsaturated carbonyl compounds to give biscyclopropane derivatives in high yield.

     

A Facile Synthesis of Indole-based Conjugated Derivatives

A novel synthetic method was developed for the preparation of indole-based conjugated derivatives with satisfied yields. By applying this strategy, a series of new compounds were prepared conveniently. All the obtained new indole derivatives were characterized by spectroscopic analyses, giving satisfactory data corresponding to their expected molecular structures.     

A Facile Synthesis of N-Protected 1-Aminoalkylphosphonamidate Derivatives

N-protected 1-amino-alkylphosphonamidates were synthesized using one-pot reactions of benzyl carbamate, aldehydes and alkoxyphosphine dichlorides and then with amines in the presence of triethylamine.     

A Facile Synthesis of Novel Benzofuranyl Benzimidazole Derivatives

In this article, we report a facile route for the synthesis of novel benzofuranyl benzimidazole derivatives. The methodology involves the Sonagashira reaction of 2‐(3‐iodo‐4‐methoxyphenyl)‐1H‐benzimidazole ( 3 ) with variety of terminal alkynes to have novel benzimidazole alkynyl derivatives followed by iodo‐cyclisation to give novel iodo benzofuranyl benzimidazole derivatives. The resulting iodo benzofuranyl benzimidazoles were functionalized further via palladium mediated carbon–carbon bond formation for molecular diversity generating novel heterocyclic compounds.     

Facile,Regioselective and Green Synthesis of Ortho‐Nitrophenoles Using NaNO2, KHSO4

Certain phenols and naphtols were nitrated regioselectively with NaNO₂ in the presence of KHSO₄ at 50 °C in high yields.     

多种形貌和晶型8-羟基喹啉铜微纳米材料的简易合成

以8-羟基喹啉和乙酸铜为主要原料,通过简单调控醇水介质和熟化时间,液相沉淀法快速合成出大量不同形貌和晶型的8-羟基喹啉铜微纳米材料.采用SEM,XRD,UV-Vis,FT-IR对产物进行表征.结果表明,以8-羟基喹啉盐酸水溶液与乙酸铜水溶液反应,合成了直径40～130nm的棒状α型二水合8-羟基喹啉铜沉淀物.以8-羟基喹啉乙醇溶液与乙酸铜乙醇溶液反应,获得了厚度约300nm的三维(3D)板条束状α型无水8-羟基喹啉铜微纳米结构.若采用8-羟基喹啉乙醇溶液与乙酸铜的乙醇/水溶液反应,当体系醇/水体积比为3∶1时,随着熟化时间的延长,产物由亚稳的α型和γ型晶相向稳定的β型晶相转变,形貌从胡须束状/菱片状混合结构转变为纳米棒状/菱片状混合结构,50min熟化后最终形成菱片状β型二水合8-羟基喹啉铜及其四角星形自组装体.     

Synthesis of Oxidized Derivatives of 10-Deuterobenzo[A]Pyrene

A series of oxidized derivatives of 10-deuterobenzol[a]pyrene (10-D-BaP) were synthesized. Oxidation of 10-D-BaP with sodium dichromate dihydrate yielded the 1,6-, 3,6-, and 6,12-quinones of 10-D-Bap. Upon electrophilic aromatic substitution of 10-D-BaP with sodium nitrate, N-bromosuccinimide, and N-chlorosuccinimide we were afforded 6-nitro-10-D-BaP, 6-bromo-10-D-BaP, and 6-chloro-10-D-BaP, respectively, in high yields. The Vilsmier-Haack reaction of 10-D-BaP provided 6-formyl-10-D-BaP which upon reduction with sodium borohydride, yielded 6-hydroxymethyl-10-D-BaP. Reduction with hydrazine in n-amyl alcohol gave 6-methyl-10-D-BaP. Reduction of 6-nitro-10-D-BaP with hydrazine and Pd/C yielded 6-amino-10-D-BaP. The synthesized compounds, which are known metabolites of benzo[a]pyrene and are useful substrates for metabolism, are important compounds for mechanistic study of the chemical carcinogenesis by benzo[a]pyrene.     

Facile Synthesis of Tris(alkoxydimethylsilyl)methane Derivatives via Alcoholysis Under Open-Flask and Mild Conditions

The reactions between a variety of functionalized alcohols and tris(dimethylsilyl)methane, (HMe₂Si)₃CH, are described. Alcohols such as ethylene glycol monobutyl ether, ethylene glycol monoethyl ether, triethylene glycol monomethyl ether, 2-chloroethanol, 1-octanol, benzyl alcohol, glycidol, and allyl alcohol were converted in the presence of Karstedt's catalyst into the corresponding tris(alkoxydimethylsilyl)methanes, (ROMe₂Si)₃CH, in a convenient one-pot operation under aerobic conditions. The appearance of the products coincides with the generation of colloidal Pt(0) species. Moreover, poly(4-chloromethyl)styrene containing tris(dimethylsilyl)methyl groups reacts with benzyl alcohol or 2-chloroethanol in the presence of Karstedt's catalyst to give new macromolecules bearing tris(alkoxydimethylsilyl)methyl groups. The reaction rate is greatly influenced by the concentration of catalyst.     

实用导向基辅助下的邻苯二酚衍生物便捷合成

5-硝基嘧啶作为导向基（DG）能很好的辅助钯催化苯酚邻位乙酰氧基化,研究发现该导向基的引入方且偶联后能在温和条件下移除。该方法操作简单,有良好的底物官能团兼容性,通过一锅法实现导向基的引入和苯酚邻位乙酰氧基化,合成了具有丰富取代基的10种2-[（5-硝基嘧啶-2-基）氧基]芳基乙酸酯新化合物。该类乙酰氧基化产物能够以最高75%收率得到,其结构均经¹H NMR, ¹³C NMR以及HR-MS（ESI）确证。     

Indium-mediated Facile Synthesis of （6-Chloropyridine-3-yl）methyl Heterocyclic Thioether Derivatives in Aqueous Media

A series of substituted (6-chloropyridine-3-yl)methyl heterocyclic thioether derivatives were prepared by indium mediating in water. The preliminary biological tests showed that compound 3d exhibited good antiviral activity.     

查尔酮衍生物E-2-(甲氨基)-7-(3-(吡啶基)丙烯酰基)卓酮的合成(英文)

以2-乙酰基-7-(甲氨基)卓酮(1)为原料,经由与各种吡啶醛的Claisen-Schmidt缩合反应得到查尔酮衍生物E-2-(甲氨基)-7-(3-(吡啶基)丙烯酰基)卓酮(2～5).全部合成产物均为新化合物,未见文献报道;其结构均由红外光谱分析、1H核磁共振、质谱及元素分析得以证实.     

Facile Synthesis of Unsymmetrical N-Aryl-2, 2-di(1H-indol-3-yl) Acetamide Derivatives

A facile and highly efficient method has been developed for the synthesis of unsymmetrical N-aryl-2,2-di(1H-indol-3-yl)acetamide derivatives by regioselective Friedel-Crafts alkylation of the N-aryl-2-hydroxy-2-(1H-indol-3-yl) acetamide derivatives with various indoles catalyzed by 2 mol/L H₂SO₄ at room temperature in a short reaction time, the yield was up to 94%.     

Synthesis and reactions of meso-(p-nitrophenyl)porphyrins

An improved methodology is reported for the regioselective nitration of the phenyl groups of meso-tetraphenylporphyrin 1, using NaNO₂ and TFA. The degree of nitration is easily controlled by the equivalent amount of NaNO₂ used and the reaction time. The nitroporphyrins are reduced to the corresponding aminoporphyrins under standard SnCl₂/HCl conditions. Reaction of tri-aminoporphyrin 9 with 1-formyl-o-carborane followed by reduction using NaBH₄ gave a novel tri-carboranylporphyrin bearing amine linkages between the porphyrin and the carborane groups.     

系列纳米结构锰氧化物的水热合成

以KMnO₄为锰源、抗坏血酸(AA)为还原剂,采用水热法制备系列纳米结构锰氧化物。通过调节反应物的物质的量的比、水溶液的pH值、反应温度和反应时间,制备出了不同纳米结构的锰氧化物,包括Mn₃O₄纳米粒子、MnOOH、α-MnO₂和β-MnO₂纳米棒。采用XRD和TEM测试技术对合成产物进行了表征,同时对其反应机理进行了探讨。     

Facile Synthesis of Novel Pentofuranose Analogs of Phospha Sugar Derivatives

Novel pentofuranose analogs of phospha sugar derivatives were synthesized starting from 1-phenyl-2-phospholene 1-oxide ( 1 ). First, the allylic oxidation of 1-phenyl-2-phospholene 1-oxide ( 1 ) with CrO 3 in Ac 2 O-AcOH or 3-hydroxy-1-phenyl-2-phospholene ( 2 ) with MnO 2 afforded 1-phenyl-4-oxo-2-phospholene 1-oxide ( 3 ). The C-5 alkylation of 3 in the presence of NaH by using benzyl bromide or methyl iodide as electrophiles afforded the target title compounds.     

Facile One-Pot Method for the Synthesis of Polysubstituted Phthalide Derivatives

A new three-component cyclization method is described involving two starting materials, ethyl 4-chloroacetoacetate and aldehydes, catalyzed by piperidine, acid, and iodine. Ten corresponding polysubstituted phthalides are formed with good yields (44–78%). A mechanism of the reaction is also proposed.