树脂D732负载磷钨酸催化合成水杨酸酯

在水杨酸和正丁醇反应中,采用强酸性阳离子树脂D732负载磷钨酸为催化剂,合成了水杨酸酯。考察了醇/酸的摩尔比、反应时间、反应温度、催化剂的用量和催化剂的重复使用性等因素对反应酯化率的影响。结果表明,在反应温度为110℃,反应时间3h,酸/醇摩尔比为1:3,催化剂质量占水杨酸总质量的20%的较优条件下,酯化率达93.2%。催化剂不经处理重复使用4次,酯化率均在83%以上。依据该较佳的工艺条件,进一步催化合成其它水杨酸酯,酯化率均超过82%,表明D732负载磷钨酸具有良好催化效果。     

锗钨酸催化合成水杨酸异戊酯

Isoamyl salicylate was synthesized by using germanotungtic acid as catalyst.The effects of the amaunt of catalyst,the molar ratio of salicycic acid of isoamy l alcohol,the reaction temperature and the reaction time on the yield of ester w ere studied.The optimum reaction conditions were 1.3∶100 (mass ratio) of cataly st to reactants,1∶2.5 (molar ratio) of acid to alcohol,135～153℃ being satisfa ctary reaction temperature and reaction time suitable being 3h.Under such condit ion,the yield of ester was up to 94%.Germanotungtic acid catalyst can be used re peatedly.     

微波辐射快速合成乙酰水杨酸

以本杨酸和乙酸酐为原料、无水碳酸钠作催化剂微波辐射快速合成乙酰水杨酸，并用正交试验筛选出最佳合成工艺条件：n(水杨酸)：n(乙酸酐)＝1：2．0，微波功率464W，辐射时间60S，催化剂用量为水杨酸质量的2％，重结晶后产率可达90．8％。     

微波协同大孔树脂催化合成肉桂酸酯的扩大实验研究(Ⅱ)

研究了微波协同大孔树脂催化合成肉桂酸正戊酯和异戊酯的扩大实验。结果显示,合成肉桂酸正戊酯的优化工艺条件为：肉桂酸7．4g,正戊醇17mL,CAT-600大孔树脂6．4g,微波功率400W,反应时间为8min时,酯化率97．23％;合成肉桂酸异戊酯的优化工艺条件为：肉桂酸7．4g,异戊醇19mL,CAT-600大孔树脂8．1g,微波功率700W,反应时间为8min时,酯化率97．01％。     

功能化酸性离子液体绿色合成酯及理论研究

实验探索了酸性功能化室温离子液体1-丙烷磺酸基-3-甲基咪唑硫酸氢盐([mimps][HSO4])催化乳酸与正丁醇、丙酸与异戊醇进行酯化反应的新工艺。考察了醇酸摩尔比、催化剂用量和反应时间等因素对酯化率的影响。结果表明,在优化工艺条件下乳酸正丁酯和丙酸异戊酯的酯化率分别为69.8%和92.1%;采用量子化学密度泛函理论计算并从热力学角度分析了二者酯化率存在较大差异的原因。生成的酯不溶于催化体系,采用分液漏斗即可实现催化剂的分离过程。离子液体循环使用10次,催化效果无明显降低。     

微波合成水杨酸异丙酯

研究了微波合成水杨酸异丙酯的工艺，与常规方法相对比，发现利用微波合成 水杨酸异丙酯具有反应速度快、转化率高、杂质含量小、后处理简单、无三废排放 等优点。     

微波协同大孔树脂催化合成肉桂酸酯的扩大实验研究(Ⅰ)

研究了微波协同大孔树脂催化合成肉桂酸正丙酯和异丁酯的扩大实验。结果表明,合成肉桂酸正丙酯的优化工艺条件为：肉桂酸7．4g,正丙醇19mL,CAT-600大孔树脂6．8g,微波功率400W,反应时间为25min,酯化率92．89％;合成肉桂酸异丁酯的优化工艺条件为：肉桂酸10g,异丁醇45mL,NKC-9大孔树脂14g,微波功率600W,反应时间为35min,酯化率90．18％。     

铁系固体酸催化剂的制备及催化合成水杨酸酯

制备了铁系固体酸催化剂(Ⅰ)并将其用于催化合成水杨酸酯，优化了反应条件：当Ⅰ用量为投料质量的6．1％，mol酸：mol醇=1：4，适当提高反应温度，合成水杨酸戊酯的反应时间可缩短至3h，产率达91．3％。合成其它水杨酸酯时也取得很高的产率。通过对比，Ⅰ的催化酯化能力优于Fe2O3／SO4^2-固体超强酸催化剂，套用6次后催化性能基本保持不变。     

氯化锡催化合成马来酸二丁酯

以SnCl4·5H2 O为催化剂 ,由马来酸酐和正丁醇合成了马来酸二正丁酯。n(马来酸酐 )∶n(正丁醇 )∶n(SnCl4·5H2 O) =1∶4∶0 .0 86 ,回流分水 6 0min ,酯收率达 92 .1% ,并用类似方法合成了收率较高的马来酸二异丁酯、马来酸二正戊酯和马来酸二异戊酯     

微波辐射合成乙酸异戊酯的工艺研究

微波辐射下以乙酸与异戊醇为原料,硫酸为催化剂合成出乙酸异戊酯,经红外光谱等表征产物是乙酸异戊酯。考察了微波作用时间、异戊醇和乙酸的摩尔比和微波功率对反应产率的影响;还通过L9(34)正交试验,确定合成乙酸异戊酯的最佳条件是异戊醇和乙酸的摩尔比为1∶3.0、微波作用时间14 min、微波功率500 W;在最优条件下的重复实验,平均产量92.6%,实验重复性好,收率较高。     

Synthesis of Substituted Salicylanilides under Microwave Irradiation

Summary. Salicylanilides were prepared in 70–95% yields in 4–8min from phenyl salicylate or phenyl 4-methoxysalicylate and substituted anilines under microwave irradiation under solvent free conditions.Received October 17, 2002; accepted October 22, 2002 Published online July 3, 2003     

微波辐射固体酸催化合成马来酸双酯

首次在微波辐射下，用活性炭固载对甲苯磺酸催化合成了马来酸双酯．当微波辐射功率为150W．正辛醇：酸酐＝3：1，催化剂用量为2．5g时，反应20min后，马来酸酐转化率达89．8％，产物的选择性为99．5％．同时，也发现随着醇的炭数增多，反应温度和反应速率增加；在微波辐射条件下，酯化反应速率、产物选择性都高于常规加热方式下的反应结果．     

Microwave Irradiation Promoted Synthesis of Aryloxy Acetic Acids

Several aryloxy acetic acids were synthesized under microwave irradiation. The factors, which affect the reaction, were investigated and optimized. It was revealed that the best yields(92. 7%--97.4%) were obtained when the molar ratio of the reactants was n(ArOH) : n(NaOH) : n(CICH2CO2H) = 1：2.5： 1.2 with microwave irradiation power of 640 W for 65--85 s.     

Synthesis of Glucosylguanidinohydrazones under Microwave Promotion and Ultrasound Irradiation

Guanylhydrazone derivatives were obtained by the condensation of glucosylated aminoguanidines with 3‐formylchromones in refluxing THF. Target compounds were synthesized by conventional method, microwave promotion and ultrasound irradiation methods. The structure of all new compounds was confirmed by IR, ¹H NMR, ¹³C NMR spectral data and elemental analyses.     

手性臂脱氧胆酸分子裂缝受体的一锅法微波合成

以脱氧胆酸为隔离基,3位构建非手性单元,12位引入手性单元,微波辐射一锅法合成具有不同手性中心和裂穴的新型手性臂分子裂缝受体,结构均经1H NMR、IR、MS及元素分析所确证。     

Synthesis of Guanylhydrazones Under Microwave Irradiation

Abstract

The reaction of aromatic aldehydes and ketones with aminoguanidine hydrochloride under microwave irradiation (MWI) afforded guanylhydrazones in shorter reaction times and improved yield as compared to the conventional methodology.     

Traceless Synthesis of Hydantoin by Focused Microwave Irradiation

Hydantoin analogs have shown versatile therapeutic applications and some of them have been approved by FDA as drugs. For example, Fosphenytoin as a sodium channel antagonist is used for the treatment of epilepsy. Phenytoin has antiarrhythmic, anticonvulsant and antineuralgic activities. Ethotoin and Mephenytoin both show anticonvulsant effect. Nilutamide is a non-steroidal orally-active antiandrogen in combination with surgical castration for the treatment of stage D2 metastatic prostate c…     

Simultaneous Synthesis of Pyrazolopyridines and Pyrazolopyrimidinones Under Microwave Irradiation

The direct reaction of o-aminopyrazocarbonitriles and carbonyl compounds to afford pyrazolopyrimidinones was discovered; hence, a simultaneous synthetic method for pyrazolopyridines and pyrazolopyrimidinones was achieved. Under microwave irradiation, better yields of products than those of conventional method were given.     

微波辐射下合成芳香硫醚

本文对在微波条件下S－烃基化反应进行了研究，并提供一种硫酚和卤代烃在氧化铝作载体的条件下，不用任何有机溶剂经微波辐射简便、快速、有效合成芳香硫醚的方法。     

嘧啶酮衍生物的微波合成

在微波辅助下,Baylis-Hillman加成物与4-氨基-6-氯嘧啶或2-氨基-噻唑反应,快速合成了两类嘧啶酮衍生物——3-取代-7-氯-4H-嘧啶[1,2-b]哒嗪-4-酮和6-取代-5H-噻唑[3,2-a]嘧啶-5-酮,收率81%～98%,其结构经1H NMR,13C NMR,IR和MS确证。