Synthesis of Thioglycosides in Room Temperature Ionic Liquid

An eco-friendly reaction for the preparation of thioglycosides has been developed using an ionic liquid as the solvent. Thioglycosides were obtained in excellent yields on treatment of per-O-acetylated sugar derivatives with thiols in the presence of boron trifluoride diethyl etherate in [Bmim][BF₄] as solvent at 20°C. Supplemental materials are available for this article. Go to the publisher's online edition of Journal of Carbohydrate Chemistry to view the free supplemental file.     

微波辐射下2-氨基-7,7-二甲基-3-乙氧羰基- 4-(2-呋喃)基-5-氧代-5,6,7,8-四氢-4H- 苯并吡喃的合成和晶体结构

标题化合物C18H21NO5是由2-呋喃亚甲叉氰乙酸酯和5,5-二甲基-1,3-环己酮在醋酸铵存在下用微波辐射反应得到,结构通过单晶X-射线衍射法确定,其晶体属三斜晶系,空间群P 睿琈r =332.36,a =11.232(2),b =13.048(2),c =13.274(3),α=105.7(1),β=95.68(2),g =109.56(1)? V=1752.4(6)3,Z=2,Dc=1.276Mg·m-1, =0.093mm-1,F(000)=704, 最终的偏离因子为R=0.0431,wR=0.0973,在分子结构中平面 1 (呋喃环) 与平面2 ((C(5)、 C(6)、C(9)、O(1))之间的二面角为 84.70°, 平面2 与平面 3 (C(1)、C(4)、C(5)、C(6)) 之间的二面角为 2.9°, 平面 1 与平面3 之间的二面角为 85.9°。吡喃环和与吡喃环合的六员环为信封式结构。     

2-氨基-4,6-二芳基吡啶的微波辐射促进合成

氯化N-氰甲基吡啶在微波辐射下于醋酸铵/醋酸体系中和4种查尔酮反应, 或直接与芳香醛和取代苯乙酮一锅煮反应, 高产率地生成了2-氨基-4,6-二芳基吡啶衍生物. 化合物的结构经过IR, ¹H NMR和HPLC-MS的表征.     

微波促进碱性离子液体催化合成查尔酮

以4-氯-1-丁醇,N-甲基咪唑和苯甲酸钠为原料,用微波法制得碱性离子液体{[OHBMIM]Ph COO(AIL)},其结构经FT-IR表征;以苯甲醛和苯乙酮为原料,AIL为催化剂,经微波促进的缩合反应合成了查尔酮(1),其结构经1H NMR和FT-IR确证。考察了AIL用量、微波功率、物料比和反应时间对1产率的影响。合成1的最佳反应条件为:AIL 1 mmol,苯甲醛5 mmol,n(苯甲醛)∶n(苯乙酮)=1.1,于微波功率140 W反应5 min,产率95.8%。AIL具有较好的循环使用性,循环使用6次,1产率没有明显降低。     

微波辐射下三组分“一锅法”合成5-芳基-1,5,6,7,8,9-六氢化-2H-吡唑[5,4-b]并喹啉-6-酮

在微波辐射下以芳醛、1,3-环己二酮或达米酮和氨基吡唑为原料, 用乙二醇作能量转移剂, 三组分“一锅法”快速合成了一系列吡唑[5,4-b]并喹啉类化合物. 该方法速度快(30～90 s), 产率高(88%～98%), 环境友好. 产物结构通过红外光谱、核磁共振谱和元素分析证实, 化合物4e的单晶经X射线衍射分析, 进一步确证了产物结构.     

微波辐射下一锅法合成2-氨基-6-溴-4-芳基-5H-茚并[1,2-b]吡啶-3-腈衍生物

以芳香醛、4-溴茚酮、丙二腈和醋酸铵为原料,分别用微波辐射和传统加热法,一步法合成7种未见文献报道的2-氨基-6-溴基-4-芳基-5H-茚并[1,2-b]吡啶-3-腈衍生物.对比两种方法,在常压下微波具有反应时间短、产率较高等特点.所有化合物均经IR,1HNMR和元素分析确定.     

Synthesis of Thia-calix[4]arene Hydroxamic Acids by Microwave Irradiation

Thia-calix[4]arene hydroxamic acids have been synthesized by partial reduction of nitro-thia-calix[4]arenes with hydrazine hydrate, Rn/Ni, and their coupling with benzoyl chloride under the influence of microwave irradiation with 90–95% yield and 3–6 min reaction time.     

Solvent-Free Synthesis of 2-Amino-3-aryl-5-substituted Thiophenes as Anti-inflammatory Agents using KF-Al2O3 under Microwave Irradiation

The synthesis of 2-amino-3-aryl-5-substituted thiophenes as anti-inflammatory agents catalyzed by KF-Al₂O₃ under microwave irradiation is reported.     

纳米钒酸铋的微波快速合成及光催化性能研究

采用微波辅助加热法以NaVO₃溶液和Bi(NO₃)₃·5H₂O的硝酸溶液为反应物,在10～40 min内合成了纳米钒酸铋粉末。利用XRD、FTIR、TEM、UV-Vis等手段研究了反应时间对产物结构及形貌的影响。经测定反应10 min时,得到纯的四方相BiVO₄,随着反应时间的延长,逐渐出现单斜相的衍射峰,当反应40 min时,获得纯的单斜相BiVO₄。同时XRD和IR结果证明了相转变的过程。TEM分析表明不同的反应时间条件下样品呈现不同的形貌。不同反应时间下获得样品的光催化性能的结果表明,微波反应时间对BiVO₄结构的转变及光催化性能的改变起到了重要的作用。     

微波辐照方式对CdS和Bi2S3纳米粒子结晶度的影响

The effect of traveling microwave irradiation on the crystallinities of CdS nanoparticles and Bi₂S₃ nanorods was studied. Results showed that as compared with stationary microwave irradiation the crystallinities and the crystal growth of sulfide nanoparticles were improved. Traveling microwave irradiation can supply narrower frequency distribution and stronger power density of irradiation， CdS nanoparticles and Bi₂S₃ nanorods obtained are better in crystallinities and larger in size than under stationary microwave irradiation.     

ZrO2 and Cu/ZrO2 Sol-Gel Synthesis in Presence of Microwave Irradiation

The sol-gel technique with a microwave irradiation was used to synthesize ZrO₂ and Cu/ZrO₂ solids at various pH values and hydrolysis catalysts. Microwave irradiation induces ZrO₂ tetragonal phase formation at almost any pH. The copper was bonded through oxygen bonds to the zirconia lattice. The introduction of copper favored the support acidity.     

Density and Refractive Index for Binary Systems of the Ionic Liquid [Bmim][BF<Subscript>4</Subscript>] with Methanol, 1,3-Dichloropropane,and Dimethyl Carbonate

Refractive indices at 298.15 K and densities in the temperature interval 293.15 to 318.15 K were determined at atmospheric pressure over the whole composition range for the binary systems [Bmim][BF₄]+(methanol, or 1,3-dichloropropane, or dimethyl carbonate). Due to the high viscosity of the samples, which would produce a wrong density if a classical vibrating-tube densimeter were used, a densimeter was employed that automatically corrects the data for the viscosity effect. Because at room temperature some [Bmim][BF₄]+dimethyl carbonate mixtures showed partial immiscibility, liquid-liquid equilibrium was determined for this system. Excess molar volumes and deviations of refractive index from linear mixing behavior were calculated from the experimental data. An erratum to this article can be found at     

A Facile Synthesis of 5-Arylidene-2-imino-4-thiazolidinones Under Microwave Irradiation

A series of 5-arylidene-2-imino-4-thiazolidinone derivatives were synthesized by the cross-aldol condensation of aromatic aldehydes with 2-imino-4-thiazolidinone in sodium acetate/acetic acid under microwave irradiation. The reactions were completed in 10 min with 63–91% yields, were environmental benign, and had easy workup.     

微波辐射下2-氨基苯并[h]喹唑啉衍生物的合成

2-芳亚甲基-3，4-二氢-2H-1（2H）-萘酮和碳酸胍在以乙二醇为溶剂、微波辐 射下反应，生成一系列新的2-氨基-4-芳基-5，6-二氢化苯并[h]喹啉衍生物，产物 的结构通过单晶X射线衍射分析确证。     

Convenient Preparation of Pyrano Benzopyranes in Aqueous Media

The three‐component reaction of aldehyde, malononitrile, and 4‐hydroxy coumarin has been efficiently performed in aqueous K₂CO₃ using a simple, clean, environmentally benign, novel procedure employing microwave irradiation. The observed yields and enhancement in reaction rates can be attributed to the uniform heating effect of microwave. The microwave‐accelerated reaction technique not only eliminates the use of external base and organic solvents but also requires only water in both the reaction step and workup, thus rendering the whole procedure into a truly ecofriendly protocol.     

单模聚焦微波辅助合成1-乙基-3-羧甲基咪唑四氟硼酸盐离子液体

以1-乙基咪唑为原料,采用discover环形单模聚焦微波合成仪合成了1-乙基-3-羧甲基咪唑四氟硼酸盐离子液体,对产品结构进行了表征及热性分析,并测定了粘度、密度、表面张力、电化学窗口等物化性能,同时考察了合成离子液体对淀粉的溶解性能.结果表明,单模聚焦微波辐射合成具有速度快、时间短、反应条件温和等优点,产品产率为88.23％,其密度、粘度、表面张力与温度均呈线性关系,且随温度升高而减小.与水溶剂相比,合成的离子液体对可溶性淀粉具有较高的溶解度,为淀粉及其衍生物的均相衍生化反应提供了理论基础.     

Synthesis of o-LiMnO2 by Microwave Irradiation and StudyIts Heat Treatment and Lithium Exchange

Microwave irradiation of a suspension of γ-MnOOH in a 4 mol dm⁻³ LiOH solution brought about a rapid formation of semicrystalline orthorhombic LiMnO₂ (o-LiMnO₂) within 30 min at 120°C. Cubic Li_1.6Mn_1.6O₄ was obtained by heating o-LiMnO₂ at 400°C; lithium could be topotactically extracted from Li_1.6Mn_1.6O₄ with acid to form cubic H_1.6Mn_1.6O₄.     

微波辐射下"一锅煮"法合成2-氨基-3-氰基-4-芳基-4H,5H-吡喃-[3,2-c]苯并吡喃-5-酮

以芳醛、4-羟基香豆素、丙二腈为原料,乙醇为能量转移剂,哌啶为催化剂,在微波辐射下一步合成了一系列2-氨基-3-氰基-4-芳基-4H,5H-吡喃-[3,2-c]苯并吡喃-5-酮,反应在40～60s时间内完成,产率60%～97%.     

Microwave Irradiation for Accelerating Synthesis of 5,6-Diphenylimidazo[1,2-a]pyrimidines Based on Isoflavones

Microwave irradiation was used to accelerate the cyclocondensation of isoflavones with 2-aminoimidazole to synthesize 5,6-diphenylimidazo[1,2-a]pyrimidines. A series of 17 new compounds were characterized by Fourier transform infrared, NMR, and elemental analysis. 5-(2-Hydroxyl-4-isopropoxyphenyl)-6-phenylimidazo-[1,2-a]pyrimidine was determined by x-ray diffraction. A variety of substrates can participate in the process with good yields and purities, making this methodology suitable for library synthesis in drug discovery.      

微波辐射下2-芳基取代苯并噁唑的合成

邻氨基酚和芳香羧酸在微波辐射条件下缩合,合成了4种2-芳基取代苯并噁唑化合物。优化反应条件为：多聚磷酸为催化剂,辐射功率500W,辐射时间4min。