三氯化镧催化一锅法合成3,4-二氢嘧啶-2-酮

二氢嘧啶酮;三氯化镧催化一锅法合成3;4-二氢嘧啶-2-酮     

A Simple and Convenient One-Pot Synthesis of Benzimidazole Derivatives Using Cobalt(II) Chloride Hexahydrate as Catalyst

A simple and efficient method for the convenient synthesis of 2-arylbenzimidazole has been described on reaction with o-phenylenediamine and various aromatic aldehydes using cobalt(II) chloride hexahydrate as a catalyst. The method is cost-effective, high-yielding, clean, and selective.     

甲烷磺酸钕催化"一锅法"合成3,4-二氢嘧啶-2-酮

在甲烷磺酸钕催化下,醛、β-二羰基化合物和脲在无水乙醇中进行环化缩合,反应条件为:醛30 mmol,β-二羰基化合物(乙酰乙酸乙酯、乙酰乙酸甲酯、戊二酮)35 mmol,脲45mmol,甲烷磺酸钕3 mmol,无水乙醇10 ml,加热回流0.5～2.0 h,通过一锅法有效地合成了高纯度3,4-二氢嘧啶-2-酮衍生物,产率69%～93%.该催化剂在反应过程中不水解,催化效率高,缩短了反应时间,且操作简便,改进了Biginelli反应.     

硝酸镧高效催化合成3,4-二氢嘧啶-2(1H)-(硫)酮

报道了以La(NO3)3催化芳香醛、β-酮酯和脲或硫脲-锅法合成3,4-二氢嘧啶-2(1H)-(硫)酮的简单、有效方法.与经典Biginelli反应条件相比,它具有产率高、反应时间短和操作简单等优点.所有目标化合物的结构经元素分析、IR、13C NMR和1H NMR确证.     

Simple,Convenient Method for the Synthesis of Substituted Furan-2(5H)-one Derivatives Using Tin(II) Chloride

Furan-2(5H)-one derivatives have been synthesized by a simple, efficient, one-pot, three-component condensation of anilines, dimethylacetylenedicarboxylate, and aromatic aldehydes in the presence of a catalytic amount of tin(II) chloride in excellent yields.     

Convenient Synthesis of Monosubstituted Arylferrocenes Using PEG-1000 as Phase-Transfer Catalyst

A new approach for the synthesis of monosubstituted arylferrocenes based on the coupling of aryldiazonium salts with ferrocene using PEG-1000 as an efficient phase-transfer catalyst was developed. The present method is applicable to many kinds of substituted aromatic amines, providing good to excellent yields of desired products.      

3-亚甲基六氢苯并呋喃-2(3H)-酮的简便合成

以氧化环己烯为原料,在正丁基锂作用下与乙腈经开环反应制得2-羟基环己基乙腈(2);2依次经水解、内酯化、二甲胺甲基化、甲基化和Hofmann降解反应合成了α-亚甲基-γ-丁内酯类化合物--3-亚甲基六氢苯并呋喃-2(3H)-酮,总收率30.4%,其结构经¹H NMR,¹³C NMR和HR-MS(EI)确证。     

A Convenient Synthesis of Aryl Phosphorodichloridothioates Using Phase Transfer Catalyst

A simple, convenient synthesis of aryl phosphorodichloridothioates using tetra-butylammonium bromide (TBAB) as phase transfer catalyst is described.     

A Convenient Synthesis of N-Substituted 1,6-Dihydro-3(2H)-Pyridinones

N-Substituted 1,6-dihydro-3(2H)-pyridinones have been synthesised from N-substituted piperidine-3,5-diones via the methyl enol ethers. Reduction of the latter with sodium borohydride (NaBH₄) is described.     

Simple and Efficient Synthesis of 2-Aryl-2,3-Dihydroquinolin-4(1H)-ones Using Silica Chloride as a New Catalyst Under Solvent-Free Conditions

A mild, efficient, and high-yielding method for the synthesis of 2-aryl-2,3-dihydroquinolin-4(1H)-ones from their corresponding 2-amino chalcones using silica chloride (SiO₂Cl) under solvent-free conditions is described. A series of 2-aryl-2,3-dihydroquinolin-4(1H)-ones containing both electron-donating and electron-withdrawing substituents were synthesized.     

A Convenient One-Pot Synthesis of Di-t-butylphosphinic Chloride

A convenient one-pot synthesis of (t-Bu)₂P(O)Cl (1) from m-chloroperbenzoic acid and (t-Bu)₂PCl is described. The byproduct m-chlorobenzoic acid is neutralized by addition of Et₃N. Complex 1 crystallizes in the monoclinic space group P2₁/c (No. 14), with a = 5.9637(2) Å, b = 11.4734(4) Å, c = 16.2400(5) Å and β = 107.7160(14).     

Zirconium(IV) Chloride Mediated Cyclodehydration of 1,2‐Diacylhydrazines: A Convenient Synthesis of 2,5‐Diaryl 1,3,4‐Oxadiazoles

Abstract

Zirconium(IV) chloride was invented as a mild catalyst for the cyclodehydration of 1,2‐diacylhydrazines. Efficient synthesis of several 2,5‐disubstituted 1,3,4‐oxadiazoles is reported.     

Synthesis of novel 3-(1,3-thiazol-2-yl)-7,8-dihydroquinoline-2,5(1H,6H)-diones

An efficient method for the synthesis of novel 3-(1,3-thiazol-2-yl)-7,8-dihydroquinoline-2,5(1H,6H)-diones from various 2-dimethylaminomethylidenecyclohexane-1,3-diones, (1,3-thiazol-2-yl)acetonitriles, and dimethylformamide dimethyl acetal was developed. These transformations proceeded through intermediate 2-[2-(4-aryl-1,3-thiazol-2-yl)-2-cyanoethenyl]-3-oxocyclohex-1-en-1-olates. They were isolated as piperidinium salts and used in further heterocyclization reactions with aromatic amines, giving novel 1-aryl-3-(1,3-thiazol-2-yl)-7,8-dihydroquinoline-2,5(1H,6H)-diones. These compounds were also obtained by preparative three-step “one pot” synthesis under controlled microwave irradiation. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 412–417, February, 2008.     

One—pot Synthesis of 3,4—dihydropyrimidin—2（1H）—one Using TsOH as a Catalyst under Microwave Irradiation

A series of Biginelli compounds was synthesized using TsOH as a catalyst under microwave irradiation.This simple method provided the title compounds in 86%-98% yields by the reaction of aromatic aldehydes with 1,3-carbonyl compound and urea.The structure of 40 was determined by single crystal Xray diffraction analysis.     

CBS催化硼烷胺配合物不对称还原法制备（S）-3-氯-1-苯基-1-丙醇

分别以R-α,α-二苯基脯氨醇、(1R,2S)-2-氨基-1,2-二苯基乙醇和(1R,2S)-(-)-1-氨基-2-茚醇为催化剂,以多种硼烷胺配合物为还原剂,由β-氯代苯乙酮不对称合成(S)-3-氯-1-苯基-1-丙醇,收率88.3%~93.8%,e.e.值为81.6%~87.7%。 用硼烷胺配合物代替硼烷-THF和硼烷二甲硫醚,稳定性好,容易计量和安全操作。     

二氧化硅负载磷钨酸催化合成3,4-二氢嘧啶-2(1H)-酮衍生物

以取代苯甲醛、乙酰乙酸乙酯和尿素为原料,以溶胶凝胶法制备二氧化硅负载的磷钨酸（H3PW12O40/SiO2）为催化剂,催化合成3,4-二氢嘧啶-2(1H)-酮,考察了三组分摩尔比、反应温度、催化剂用量及反应时间对反应收率的影响。 研究表明,H3PW12O40/SiO2是合成3,4-二氢嘧啶-2(1H)-酮的良性催化剂,在取代苯甲醛的用量为0.04 mol,反应温度为90 ℃的条件下,收率可达73.1%~88.4%。 催化剂和产品结构分别经IR、XRD、SEM和1H NMR、IR、MS等技术手段表征。     

活性炭固载氯化铁催化合成柠檬酸三丁酯

研究了以活性炭固载氯化铁为催化剂 ,柠檬酸和正丁醇为原料合成柠檬酸三丁酯 ,通过正交试验和单因素检验确定了最佳合成条件 ,结果表明 :当柠檬酸用量为 0 .1mol时 ,正丁醇用量为 0 .5mol,催化剂用量为 4g ,在回流温度控制反应时间为 2h ,其酯化率可达 95 .7%     

Synthesis of 3-Dipeptidyl-2,4(1H,3H)-Quinazolinediones as Potential Anti-Hypertensive Agents

Quinazolinediones bearing a dipeptide side chain have been synthesized as potential anti-hypertensive agents.     

Synthesis of 3-amino-2,4(1H,3H)-quinazolinediones for testing as anticonvulsants

A number of 3-amino-2,4(1H,3H)-quinazolinediones were synthesized from o-aminobenzoylhydrazines and ethyl chloroformate in pyridine or from 2-methoxycarbonylphenyl isocyanate and 1,1-disubstituted hydrazines. Four of the ten compounds screened exhibited anticonvulsant activity in mice.