Ferric Sulphate Hydrate–Catalyzed,Microwave‐Assisted Synthesis of 2,3‐Unsaturated O‐Glycosides via the Ferrier Reaction

Fe₂(SO₄)₃ · xH₂O catalyzes the Ferrier reaction of per‐O‐acetylated/benzylated glycals with alcohols to give 2,3‐unsaturated α‐glycosides in a few minutes under microwave irradiation.     

Facile Preparation of Benzylic Iodides Under Solvent‐Free Conditions Using Microwave Irradiation

Abstract

Benzylic alcohols are rapidly converted to the corresponding benzylic iodides using combination of p‐toluenesulfonic acid (PTSA) and potassium iodide under solvent‐free microwave irradiation conditions.     

Facile Synthesis of Pyrano[2,3‐c]pyrazol‐6‐one Derivatives Under Microwave Irradiation in Solvent‐Free Conditions

A series of substituted 1H,6H‐pyrano[2,3‐c]pyrazol‐6‐one derivatives were synthesized from one‐pot cyclocondensation of hydrazine derivatives or 1H‐pyrazol‐5‐one derivatives with various β‐keto esters under solvent‐free conditions using microwave irradiation in short time with good to excellent yields.     

One‐Pot Synthesis of Iminoimidazolines under Microwave Irradiation in Solvent‐Free Conditions

Substituted iminoimidazolines were synthesized from a one‐pot reaction of aromatic or hetero‐aromatic amines with imidazolidine‐2‐thione under solvent‐free conditions using microwave irradiation with good to excellent yields.     

Synthesis of 2‐Substituted 4,5‐Diphenyloxazoles under Solvent‐Free Microwave Irradiation Conditions

A novel method for the direct conversion of deoxybenzoin into 2‐alkyl‐4,5‐diphenyloxazoles and 2‐aryl‐4,5‐diphenyloxazoles has been developed using treatment of HTIB and nitriles under solvent‐free microwave irradiation conditions.     

Amberlyst 15–Catalyzed Efficient Synthesis of 2,3‐Unsaturated Glycosides via Ferrier Rearrangement for Glycal

Amberlyst 15 serves as an inexpensive, effective, and environmentally friendly catalyst in converting 3,4,6‐tri‐O‐acetyl‐D‐glucal (1) into 2,3‐unsaturated O‐ and S‐glycosides via Ferrier rearrangement in moderate to excellent yields with high α selectivity.     

Microwave‐Assisted Ring Opening of Epoxides in Solvent‐Free Conditions

The reaction of aryloxymethyl epoxide with anilines under solvent‐free conditions and microwave irradiation affords high yields of 1‐arylamino‐3‐aryloxypropan‐2‐ols. The reaction was rapid and completely regioselective.     

Microwave‐Assisted Synthesis of Amide under Solvent‐free Conditions

An efficient and environmentally friendly synthetic method for the synthesis of primary amides under microwave irradiation was described, in which the primary amine was directly reacted with acid without any catalytic agents. The reaction took place in 8–12 min, which was much shorter than the traditional synthetic methods, with almost quantitative yields. The influential factor of the reaction was discussed. The tautomerization between the carboxylic acid group and the H atom in α‐carbon of L‐amino acid was observed, presumably a dehydrated intermediate forming from this tautomerized isomer.     

Efficient Synthesis of Phosphono‐ and Phosphinoxidomethylated N‐Heterocycles under Solvent‐Free Microwave Conditions

Simple N‐heterocycles were converted to N‐phosphono‐ and phosphinoxidomethyl derivatives by a solvent‐free microwave‐assisted condensation of the heterocycle, paraformaldehyde, and diethylphosphite or diphenylphosphine oxide in a convenient and, in most cases, efficient way. In contrast to an earlier report, imidazole proved to be unreactive in this type of phospha‐Mannich reaction.     

PEG‐SO3H as Catalyst for 3,4‐Dihydropyrimidones via Biginelli Reaction Under Microwave and Solvent‐Free Conditions

An efficient and environmentally friendly process for the synthesis of 3,4‐dihydropyrimidones via the Biginelli‐type condensation reaction using poly(ethylene glycol)‐bound sulfonic acid as catalyst irradiated by microwave has been developed. The functionalized poly(ethylene glycol) acted simultaneously as catalyst and as solvent in the condensation. The workup was easy, and the products were obtained in good to excellent yields and high purities.     

Microwave‐Assisted Protection of Phenols as tert‐Butyldimethylsilyl (TBDMS) Ethers Under Solvent‐Free Conditions

Abstract

A facile, time‐saving procedure to protect phenols with tert‐butyldimethylsilyl chloride using imidazole as catalyst under solvent‐free conditions is described. Several phenolic compounds with different substitution patterns can be silylated in high yield with substantially reduced generation of residues, a present goal in organic synthesis.     

Microwave‐Assisted Efficient Synthesis of Dihydropyrimidines in Solvent‐Free Condition

Abstract

An efficient synthesis of 3,4‐dihydropyrimidinones from an aldehyde, a ketoester, and a urea or thiourea using a catalytic amount of ferric chloride hexahydrate is described. Microwave irradiation has been used to accelerate the synthesis of the Biginelli compounds under solvent‐free conditions and in a short reaction time and with good yield.     

A Facile and Efficient Synthesis of Arylsulfonates and Arylsulfonyl Hydrazides under Solvent Free Conditions

Organosulfur compounds are useful materials and most of them have pharmacological properties. The sulfonic esters are important intermediates in organic synthesis and used as acaricides and thermal recording materials. The sulfonyl hydrazides are valuable as inhibitors, agrochemical fungicides, insecticides and photographic images. Some methods have been reported for preparing these compounds to date. Usually, these reactions were carried out in organic solvent[1,2]such as pyridine and DMF. Even up-to date solid-phase synthesis requires solvent. What's more, they have other drawbacks including long reaction time, producing much wastes and by-products, tedious experimental procedure.     

Efficient Synthesis of tert‐Butyl Ethers under Solvent‐Free Conditions

A simple and efficient synthesis of tert‐butyl ethers from various alcohols and substituted phenols using tert‐butyl bromide in the presence of basic lead carbonate as a catalyst. The catalyst is easily recovered via filtration and can be reused up to three times without appreciable loss of activity.     

Facile Ionic Liquids-Promoted One-Pot Synthesis of Polyhydroquinoline Derivatives under Solvent Free Conditions

In recent years, much attention has been directed towards the syntheses of 1,4-dihydropyridyl compounds due to the fact that 1,4-dihydropyridyl compounds possess a variety of biological activities.[1] In view of the importance of polyhydroquinoline derivatives, many classical methods for the synthesis of polyhydroquinoline derivatives were reported[2] by conventional heating and refluxing approaches in the presence of organic solvent. These methods, however, involve long reaction time, harsh reaction conditions, the use of a large quantity of organic solvent and unsatisfactory yields. Therefore,improvements in such syntheses have been sought continuously.     

InCl3 as an Efficient Catalyst for Cyclotrimerization of Aldehydes: Synthesis of 1,3,5‐Trioxane Under Solvent‐Free Conditions

1,3,5‐Trioxanes derived from aldehydes were synthesized using indium trichloride as a catalyst. Cyclotrimerization of the aldehydes gave excellent yields under neat conditions within a short span of time.     

Microwave‐Assisted Solvent‐Free Regiospecific Synthesis of 5‐Alkylidene and 5‐Arylidenehydantoins

Hydantoins have become a well‐known class of structures that have found significant applications as agrochemicals and therapeutics. This structural motif is of interest in the synthesis of small building blocks suitable for the preparation of potentially bioactive molecules. In this sense, 5‐alkylidene and 5‐arylidenehydantoins constitute nice examples of precursors of synthetic α‐amino acids. The microwave‐assisted synthesis of these compounds under green chemistry conditions is reported in this article. The method has proved to afford yields of 74–96%.     

Lithium Perchlorate Mediated Three‐Component Preparation of α‐Aminonitriles Under Solvent‐Free Conditions

Abstract

A three‐component reaction between aliphatic or aromatic aldehyde, an amine and trimethylsilyl cyanide mediated by solid LiClO₄, gave amino nitriles in good to excellent yields. The reaction proceeded smoothly under solvent‐free conditions without any side products.     

Microwave‐Assisted One‐Pot Preparation of Tetrahydro‐β‐carboline Hydrochlorides under Solvent‐Free Conditions

An efficient and environmentally friendly synthesis of tetrahydro‐β‐carboline hydrochlorides via Pictet–Spengler reaction was described. Tryptamine hydrochlorides were used as the reactant and no additional acid catalyst was needed. This reaction was completed within 2.5–9 min in good yield.     

Facile Deprotection of Aromatic tert‐Butyl and Allylic Esters Under Microwave Irradiation Conditions

Abstract

A simple and efficient method for the deprotection of tert‐butyl and allylic esters is described, which occurs under microwave irradiation with p‐toluenesulfonic acid in solvent‐free conditions.