N-Sulfonic acid poly(4-vinylpyridinium) chloride as a highly effcient and reusable catalyst for the Biginelli reaction简

A mild, simple and efficient procedure for the preparation of 3,4-dihydropyrimidin-2（1H）-ones and -thiones is described using N-sulfonic acid poly（4-vinylpyridinium） chloride （NSPVPC） as a heterogeneous and efficient catalyst under solvent-free conditions. Simple methodologies, easy work-up procedure, easy preparation of the catalyst, excellent yields and very short reaction times are among the other advantages of this work. Further, the catalyst can be reused and recovered for several times without significant decrease in its activity.     

Iodine-catalyzed Efficient Synthesis of β-Keto Esters from Aldehydes and Ethyl Diazoacetate Under Solvent-free Conditions

An efficient procedure for the synthesis of β-keto esters from the reaction of aldehydes and ethyl diazoa-cetate catalyzed by iodine at room temperature under solvent-free conditions has been described. The catalytic procedure has the advantages of easily available catalyst,mild reaction conditions,high yields,and easy work-up.     

H5PW（10）V2O40催化高效环保合成14-芳基-14H-二苯并[a,j]氧杂蒽（英文）

A rapid and efficient procedure for the preparation of various aryl-14H-dibenzo[a,j]xanthenes was reported.The method developed produced excellent yields via one-pot condensation of β-naphthol with various aryl-aldehydes in the presence of Keggin vanadium substituted heteropolyacid,H5PW10V2O40,as catalyst under solvent free conditions.The present methodology therefore offered several advantages but not limited to excellent yields(82%-98%),short reaction times(30-50 min),mild reaction conditions,simple work-up,as well as the utilization of cheap and environmentally benign catalyst in the absence of organic solvents.     

H_5PW(10)V_2O_(40)催化高效环保合成14-芳基-14H-二苯并[a,j]氧杂蒽(英文)

A rapid and efficient procedure for the preparation of various aryl-14H-dibenzo[a,j]xanthenes was reported.The method developed produced excellent yields via one-pot condensation of β-naphthol with various aryl-aldehydes in the presence of Keggin vanadium substituted heteropolyacid,H5PW10V2O40,as catalyst under solvent free conditions.The present methodology therefore offered several advantages but not limited to excellent yields(82%-98%),short reaction times(30-50 min),mild reaction conditions,simple work-up,as well as the utilization of cheap and environmentally benign catalyst in the absence of organic solvents.     

Highly efficient and green synthesis of 14-aryl(alkyl)-14H-dibenzo[a,j]xanthene and 1,8-dioxooctahydroxanthene derivatives catalyzed by reusable zirconyl triflate [ZrO(OTf)2]under solvent-free conditions

An efficient,convenient and green method has been introduced for the preparation of 14-aryl（alkyl）-14H-dibenzo[a,j]xanthene and 1,8-dioxooctahydroxanthene derivatives by the reaction of aldehydes with 2-naphthol and 5,5-dimethyl-1,3-cyclohexanedione, respectively,in the presence of ZrO（OTf）₂ as a reusable catalyst under solvent-free conditions.In addition,very short reaction times, excellent yields,straightforward procedure,and relatively non-toxicity of the catalyst are other noteworthy advantages of the present method.     

硅胶键合的N-丙基三亚乙基四胺氨基磺酸作为可回收固体酸催化剂催化合成2-氨基-4,6-二芳基烟腈(英文)

A simple and efficient procedure for the preparation of silica-bound N-propyl triethylenetetramine sulfamic acid(SBPTETSA) by the reaction of silica-bound N-propyl triethylenetetramine(SBPTET) with chlorosulfonic acid in chloroform is described.Silica-bound N-propyl triethylenetetramine sulfamic acid was employed as a recyclable catalyst for the synthesis of 2-amino-4,6-diarylnicotinonitriles from the multi-component reaction of an acetophenone derivative,an aromatic aldehyde,malononitrile,and ammonium acetate under solvent-free conditions at 100 °C.The heterogeneous catalyst was recycled for five consecutive runs in the optimized multi-component reaction of 4-chloroacetophenone,4-chloroenzaldehyde,malononitrile,and ammonium acetate without significant loses to its catalytic activity.     

无溶剂条件下碳基固体酸催化一锅法合成酰胺烷基萘酚(英文)

An efficient, environmentally friendly procedure for the synthesis of amidoalkyl naphthols through the one‐pot, three‐component reaction of β‐naphthol, aryl aldehydes, and acetamide in the presence of a carbon‐based solid acid under thermal solvent‐free conditions is described. The beneficial fea-tures of this new synthetic approach include short reaction time, high yields, clean reaction profiles, and a simple work‐up procedure. Furthermore, the catalyst can be readily recycled and reused four times without obvious significant loss of activity. The structure of the catalyst was confirmed by Fourier transform infrared spectroscopy, N2 adsorption/desorption analysis, and X‐ray diffraction.     

磺化碳催化Biginelli反应一锅法合成3,4-二氢-2(1H)-酮和硫酮(英文)

A sulfonated carbon material was shown to be a highly efficient,eco-friendly,and recyclable solid acid catalyst for the Biginelli reaction of β-ketoester,aldehyde,and urea or thiourea under solvent-free conditions.It gave 3,4-dihydropyrimidin-2(1H)-ones and-thiones in good to excellent yields.This method has the advantages of a simple procedure with easy work-up,short reaction time,and high yields.The catalyst can be recycled after a simple work-up and was reused four times without substantial reduction in activity.     

溴化镁催化的1,2,3,4-四氢吡啶酮无溶剂合成研究

An efficient and environmentally friendly procedure for the one-pot synthesis of tetrahydropyrimidinones from aldehydes, β-diketones and urea/thiourea by using magnesium bromide as an inexpensive and easily available catalyst under solvent-free conditions was described. Compared with the classical Biginelli reaction conditions, this new method has the advantage of good to excellent yields (74%-94%) and short reaction time (45-90 min). The structure of the Biginelli reaction product from β-diketone, salicylaldehyde and urea has been proposed to possess an oxygen-bridge by cyclization (intramolecular Michael-addition).     

Al(HSO4)3/ silica gel as a novel catalytic system for the ring opening of epoxides with thiocyanate anion under solvent-free conditions

<正>For the first time,metal hydrogen sulfates and phosphates/silica gel have been studied as efficient and powerful solid acid catalysts in the ring opening of epoxides with thiocyanate anion.The most significant result was obtained by Al(HSO_4)_3/SiO_2 which afforded the corresponding β-hydroxy thiocyanates under mild reaction conditions and in very short reaction times.The cheapness, availability of the catalyst,ease of procedure and work-up make this method attractive for the organic synthesis.     

Silica supported perchloric acid(HClO4-SiO2):A mild,reusable and highly efficient heterogeneous catalyst for the synthesis of axidoalkyl naphthols

An efficient and direct procedure has been developed for the preparation of amidoalkyl naphthols by a one-pot condensation of aryl aldehydes,2-naphthol and urea or amides,in the presence of HClO4-SiO2 as a heterogeneous catalyst.The reactions were carried out under reflux and solvent-free conditions.The present methodology offers several advantages such as excellent yields,simple procedure,easy work-up and ecofriendly reaction condition.The catalystis easily prepared,stable,reusable and efficient under the reaction conditions.     

Silica-supported Preyssler nano particles: a green,reusable and highly efficient heterogeneous catalyst for the synthesis of carbamatoalkyl naphthols

Abstract

An efficient and green procedure has been developed for the preparation of carbamatoalkyl naphthols by the one-pot condensation of aryl aldehydes, β-naphthol, and methyl carbamate in the presence of silica-supported Preyssler nano particles as a heterogeneous catalyst under solvent-free conditions. The present methodology offers several advantages such as excellent yields, simple procedure, easy work-up, and eco-friendly reaction conditions. The catalyst is easily prepared, stable, reusable, and efficient under the reaction conditions.     

Al(HSO4)3: an efficient and heterogeneous reusable catalyst for the synthesis of 1-amidoalkyl-2-naphthols under thermal solvent-free conditions

An efficient green protocol for the synthesis of 1-amidoalkyl-2-naphthols using a three-component, one-pot condensation reaction of 2-naphthol, aromatic aldehyde and amides in the presence of Al(HSO₄)₃ as heterogeneous catalyst under thermal solvent-free conditions has been described. The present procedure offers advantages such as shorter reaction times, simple work-up procedure, excellent yields, recovery and reusability of catalyst.     

Solvent-free synthesis of dihydropyrimidinones catalyzed by alumina sulfuric acid at room temperature

A simple, efficient and practical procedure for the Biginelli reaction using alumina sulfuric acid (ASA) as a novel acid catalyst is described under solvent-free conditions. The catalyst exhibited remarkable reactivity at room temperature. The method offers several advantages including high yields, environmentally friendly procedure, short reaction times and simple work up procedure.     

One-pot synthesis of dihydropyrimidiones catalyzed by strontium(II) triflate under solvent-free conditions

A simple, efficient and practical procedure for the Biginelli reaction using strontium(II) triflate [Sr(OTf)₂] as a novel catalyst is described under solvent-free conditions in high yields. The catalyst exhibited remarkable reactivity and it is reusable. Some of dihydropyrimidiones showed strong pesticidal activity.     

聚(4-乙烯基吡啶丁烷磺酸)硫酸氢盐:一个高效的多相聚(离子液体)固体酸催化剂用于无溶剂条件下一锅法合成1-酰氨基-2-萘酚和取代喹啉(英文)

Poly(4-vinylpyridinium butane sulfonic acid) hydrogen sulfate has been used as an efficient dual acidic catalyst for the one-pot preparation of 1-amidoalkyl-2-naphthols and substituted quinolines under solvent-free conditions.The catalyst was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, and thermo-gravimetric analysis. The results revealed several advantages to our new catalyst system,including its reusability,facile work-up procedure, eco-friendly reaction conditions,short reaction time,and high product yields.     

Hydroxyl ammonium ionic liquid-catalyzed simple and efficient synthesis of 5-arylidene-2,4-thiazolidinediones under solvent-free conditions

A simple and efficient synthesis of 5-arylidene-2,4-thiazolidinediones by the Knoevenagel condensation of aldehydes with 2,4-thiazolidinedione in the presence of 2-hydroxy ethylammonium propionate under solvent-free conditions is described. The attractive features of this procedure are operational simplicity, high yields, short reaction times, easy to prepare the catalyst, mild and environmentally benign reaction conditions, and recycle of the catalyst.     

One-pot oxidant-free dehydrogenation-Knoevenagel tandem reaction catalyzed by a recyclable magnetic base-metal bifunctional catalyst

A new base-metal bifunctional catalyst NH-Pd(0)@MNP was prepared via a facile procedure and fully characterized. The as-prepared catalyst was used as an efficient relay catalyst for the one-pot oxidant-free dehydrogenation-Knoevenagel condensation tandem reaction from benzyl alcohol in H₂O under mild conditions and generated benzalmalononitriles with yield up to 96%. Meanwhile, the catalyst could be easily recovered from the reaction system by an external magnetic field, and is reusable with little loss of activity up to 6 runs (<5%).