A Microwave Assisted Diazo Coupling Reaction: The Synthesis of Alkylazines and Thienopyridazines

Heating diazoaminobenzene with active methylene compounds 1–3 in microwave oven in acetic acid, in the presence of hydrochloric acid, afforded the corresponding arylhydrazones 5–7. These reaction products were condensed with ethyl cyanoacetate in a domestic microwave oven after 1–2 minutes heating to yield the pyridazinones 8–12. Compounds 8c and 12 reacted with sulfur in basic DMF solution, in microwave oven using MORE technology to yield the thienopyridazinone 14 and 16 respectively. While 17 was produced when 8b was treated like wise with sulfur and DMF in the presence of piperidine. Compounds 16 coupled with aromatic diazonium salts to yield arylazo derivatives 21a–c.     

Microwave‐Assisted NiCl2 Promoted Acylation of Alcohols

Abstract

A microwave oven acylation of alcohols by carboxylic acid anhydrides has been developed. NiCl₂ has been proven an efficient catalyst for the acylation of primary, secondary, and tertiary alcohols and phenols under microwave conditions.     

A fast synthesis for Zintl phase compounds of Na3SbTe3, NaSbTe2 and K3SbTe3 by microwave irradiation

The microwave irradiation technique was used to prepare three Zintl phase compounds Na₃SbTe₃, NaSbTe₂ and K₃SbTe₃. The as-prepared products were analyzed and characterized by XRD, EDX and SEM techniques. Higher microwave oven power and shorter irradiation time are required for the synthesis of Na₃SbTe₃, whereas lower oven power and longer irradiation time are needed for NaSbTe₂. Moderate microwave irradiation conditions facilitate the formation of pure K₃SbTe₃. Pure phase of Na₃SbTe₃ are directly obtained by this technique for the first time. Compared with the traditional high-temperature solid-state synthesis, the microwave reaction required a considerable shortened reaction time for the preparation of the three Zintl compounds. The initial driving force for these reactions originates from the interaction of microwave electric field with alkali metals (Na and K) and Sb powders.     

SYNTHESIS OF 4,9-DIMETHYL-8- (6-ARYL-2-THIOXO-1,2,3,6-TETRAHYDRO PYRIMIDIN-4-YL)-FURO[2,3-H]CHROMEN-2-ONES AS ANTIMICROBIAL AGENTS UNDER MICROWAVE IRRADIATION

Acrolyl furochromen-2-ones (3a–i) obtained in good yields on microwave irradiation of furochromen-2-one (1) with various simple and substituted aromatic aldehydes (2a–i). 3a–g on cyclo dehydration with thiourea in domestic microwave oven furnished tetrahydro thiaxopyrimidine furochromen-2-ones 4a–i in high yields. The structures of the newly synthesized compounds were established on the basis of analytical and spectral data, IR, and ¹H NMR.     

Green technologies in organic synthesis: self-condensation of enamines,enaminones and enaminoesters under microwave irradiation in ionic liquid

Abstract

Utilizing green technologies as microwave (MW) irradiation and ionic liquids (ILs), we could produce 1,3,5-trisubstituted benzene 3, 7, 9, and 14 by self-condensation of enamines 1, enaminones 4, 8, and enaminoester 10, respectively, in the presence of pyridinium chloride ([PyH]Cl) for short time. Also, we synthesized pyridine derivatives 17, upon irradiating enaminones 4 in domestic MW oven for short time.     

Microwave-Assisted Solvent Extraction of Melamine from Seafood and Determination by Gas Chromatography–Mass Spectrometry: Optimization by Factorial Design

Melamine attracts considerable attention because of its toxicity. The determination of melamine in seafood was performed by gas-chromatography–mass spectrometry, using an optimized version of a method adopted by the U.S. Food and Drug Administration. The melamine was extracted by closed-vessel microwave-assisted solvent extraction (MAE), as a valid alternative in sample preparation, to reduce analysis time and provide less ambiguous data. The procedure was optimized by means of experimental factorial design considering the three main variables that affect this process: microwave oven power, the maximum temperature inside the extraction tube, and the hold time. The recovery of melamine in spiked samples was used as the elemental response value of the design. Temperature and hold time had a more positive effect on the response than the microwave power. A significant positive interaction was observed between oven power and hold time. A temperature of 70°C and a hold time of 1 min gave a recovery of 92 ± 5% for a microwave power of 600 W. Under these conditions, the total microwave extraction time was approximately 2 minutes, a much shorter time compared to the ultrasonic bath, which required a total time of 40 min. The repeatability of the method was approximately 3%. The limits of quantification were 0.55 mg kg^?1 for MAE and 1.9 mg kg^?1 for the ultrasonic bath; the linearity was confirmed up to 10 mg kg^?1. In conclusion, the MAE procedure was shown to be an excellent alternative to the official method.     

A Comparison of Sample Preparation Procedures for the Determination of Iron and Zinc in Bulgur Wheat by Graphite Furnace Atomic Absorption Spectrometry

ABSTRACT

A comparison was made of different digestion methods for the determination of iron and zinc in two types of bulgur wheat prior to their analysis in graphite furnace atomic absorption spectrometry. Samples were digested by means of acid treatment in room temperature, acid treatment at 60°C in a water bath and in a microwave oven and by dry ashing in open ah system. Except for microwave digestion, the samples proved to be unclear. The concentrations of the elements studied in the bulgur samples obtained by the four digestion methods are inconsistent in limits of standard deviations. It was found that aluminum sulfate (4μg/10μl sample) added to the samples acted as a modifier, improving the signal shape and increasing the stability of slurries obtained from digestion procedures.     

Rapid and Efficient Microwave‐Assisted Synthesis of N‐Carbamoyl‐L‐amino Acids

A rapid and efficient method for the synthesis of N‐carbamoyl‐L‐amino acids is reported. The procedure, involving the reaction between urea and α‐amino acids sodium salts, was performed under microwave conditions using an unmodified domestic microwave oven. A careful study of the operative conditions indicated proline (1d) as the less reactive substrate and phenylglycine (1e) as the more reactive one among all the α‐amino acids tested. Substitution of urea with potassium cyanate produced a low conversion into the corresponding N‐carbamoyl derivative, and a possible explanation of this result is reported.     

Dehydration of sodium carbonate monohydrate with indirect microwave heating

In this study, dehydration of sodium carbonate monohydrate (Na₂CO₃·H₂O) (SCM) in microwave (MW) field with silicon carbide (SiC) as an indirect heating medium was investigated. SCM samples containing up to 3% free moisture were placed in the microwave oven. The heating experiments showed that SCM is a poor microwave energy absorber for up to 6 min of irradiation at an 800 W of microwave power. The heat for SCM calcination is provided by SiC which absorbs microwave. The monohydrate is then converted to anhydrous sodium carbonate on the SiC plate by calcining, i.e. by removing the crystal water through heating of the monohydrate temperatures of over 120 °C. The calcination results in a solid phase recrystallization of the monohydrate into anhydrate. In the microwave irradiation process, dehydration of SCM in terms of indirect heating can be accelerated by increasing the microwave field power.     

Optimized microwave preparation procedure for the elemental analysis of aquatic sediment

 This paper summarizes several key points in applying the microwave preparation technique to the elemental analysis of aquatic sediments and reports systematic experiments in searching for an optimal microwave preparation procedure for element analysis in sediment samples. The determination of the elements Cu, Pb and Cd in a standard reference aquatic sediment sample (CRM 280, COMEUR) was achieved by first digesting the samples in a microwave oven equipped with PFA advanced composite vessels, followed by AAS measurement. The influence of microwave power, digestion time, various dissolution reagents and the HF removing conditions was studied. It has been shown that for a 0.1 g sediment sample the optimal microwave preparation conditions are: 4–5ml HNO₃/HF/H₂O₂ as solvent, digesting time 30 min with 100% microwave power and evaporating the residual acid within 8 min in an open vessel at 80 °C. The element recovery rates with AAS measurement can reach up to 92.4–100.6%. Received: 23 July 1996/Revised: 23 September 1996/Accepted: 25 September 1996     

Microwave-assisted addition of azomethines to isatoic anhydride

Diels-Alder addition of azomethines to isatoic anhydride in a solvent-free and eco-friendly condition is investigated using a microwave oven. The product is exclusively 2,3-diaryl-2,3-dihydroquinazolin-4(1H)-ones 4a-d. HOMO-LUMO energy of the iminoketene and the dienophiles were calculated using semi-empirical AM1 calculations.     

Microwave‐Assisted Rapid Deacetalation of Carbohydrates

Abstract

A simple and fast procedure to deprotect carbohydrate 4,6‐di‐O‐benzylidene acetals was accomplished by using domestic microwave‐oven irradiation in solvent‐free conditions and with silica‐gel‐supported reagents.     

Characterization and Comparative Studies on Conventional and Microwave Synthesis of Some Disulfides

Abstract

Some disulfide derivatives have been prepared by microwave assisted synthesis methodology from thiophthalimides(sulfenimides) and thiols in a modified microwave oven under reflux at 600 Watt in ethanol. Elucidation of the structures of the synthesized compounds has been performed by IR, ¹H NMR, and ¹³C NMR spectroscopic methods.

[Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental files: Additional figures]     

A Microwave Digestion Method for Total Decomposition of Lead and Other Metals in Paint,Soil and Dust

ABSTRACT

A simple, total decomposition method for lead and other metals in paint has been developed. Complete decomposition is achieved through a combination of reagents over several digestive steps in a microwave oven. Results of analysis of several NIST paint SRMs show excellent recoveries ranging from 85.5 to 111%. Additionally, recoveries of a number of trace elements for two soil and one dust NIST SRM were also excellent.     

A Convenient Method for Protection and Deprotection of Alcohols and Phenols as Alkylsilyl Ethers Catalyzed by Iodine Under Microwave Irradiation

Abstract

Irradiation of alcohols or phenols with tert-butyldimethylsilyl chloride (TBDMSCl) or trimethylsilyl chloride (TMSCl) in presence of catalytic amount (20 mol%) of iodine in a microwave oven for 2 min gives the corresponding silyl ethers in excellent yield. Iodine in methanol deprotects the silyl ether into its parent alcohol or phenol under similar reaction conditions.     

Determination of Cadmium in Plant Tissues by Electrothermal Atomisation Atomic Absorption Spectrometry with Matrix/Analyte Modification and Smith-Hieftje Background Correction

Abstract

Pressure decomposition in a microwave oven provides a rapid means of sample preparation for plant tissue analyses. The use of delayed atomisation cuvettes, Smith-Hieftje background correction and matrix/analyte modification enables accurate determinations of cadmium concentrations in plant materials to be made. However, care should be taken to restrict the concentrations of modifier used, as too high a concentration may lead to problems with both tube life and over-correction by the Smith-Hieftje background correction system.     

Extraction and Quantitation of Polyolefin Additives

Abstract

The extraction and subsequent separation and quantitation of polymer additives in polyolefins has proven to be a challenge for the analytical chemist. There have been several workers over the years who have investigated the separation of additives in polyolefins (1–7), but the extraction and recovery (at > 90%) in reasonable times has been most difficult. the Soxhlet extraction technique has been used for many years, but suffers in that it takes over twelve hours to extract most of the additives used in polyolefin formulations. Some workers have used the ultrasonic bath (7), but not very much work has been done with the microwave oven. We have investigated some ways to extract the additives from polyolefins, namely, microphye oven and ultrasonic bath techniques for high density polyethylene (HDPE), low density polyethylene (LDPE), and polypropylene. We have concentrated on identifying and quantitating recoveries for typical polyolefin

antioxidants, 20 such as Irganox 1010, Irgafors 68, and Cyasorb UV 531. the extraction times are typically 20 minutes for the microwave oven and 30–60 minutes for the ultrasonic bath with 90+% recoveries being obtained. Both normal phase isocratic (used when phosphites are present) and reverse phase gradient LC techniques are discussed. We have also extracted the slip agent, erucamide, from LDPE, using reverse phase, at 200nm.     

Synthesis and characterization of CaBi4Ti4O15 thin films annealed by microwave and conventional furnaces

CaBi₄Ti₄O₁₅ thin films were deposited by the polymeric precursor method and crystallized in a domestic microwave oven and conventional furnace. The films obtained for microwave energy are well-adhered, homogeneous and with good specularity when treated at 700 ^°C for 10 min. The microstructure and the structure of the films can be tuned by adjusting the crystallization conditions. When microwave oven is employed, the films presented bigger grains with mean grain size around 80 nm. For comparison, films were also prepared by the conventional furnace at 700 °C for 2 h.     

Environmental remediation by an integrated microwave/UV illumination technique: VI. A simple modified domestic microwave oven integrating an electrodeless UV-Vis lamp to photodegrade environmental pollutants in aqueous media

A simple device is described based on a modified domestic microwave oven that incorporates an UV-Vis lamp encased in Teflon to photodegrade environmental pollutants in aqueous media. The performance of this device was examined using the photodegradation of the agrochemical pollutant 2,4-dichlorophenoxyacetic acid (2,4-D) as the test process driven by a coupled photocatalytic/microwave method in an aqueous TiO₂ dispersion. The aqueous dispersion was contained in a high-pressure Teflon batch (TB) reactor that also integrated a double glass cylindrical plasma lamp (DGCPL) as the source of the UV-Vis radiation. This DGCPL lamp contained mercury gas with a minute amount of neon gas and was powered solely by microwave radiation. The coupled microwave-UV-Vis irradiation of the TB-DGCPL reactor led to an enhancement of the decomposition of the 2,4-D target substrate in the modified microwave oven relative to the photocatalytic method alone. Specifically, the rates of degradation were 2×10⁻³ mM min⁻¹ (photocatalytic/microwave method (PD/MW)) and 1.1×10⁻³ mM min⁻¹ (photocatalytic method (PD)) even though the light irradiance was some six-fold greater in the latter method. That is, the coupled PD/MW method was about 10 times more efficient than the PD method alone.     

Druckaufschlu? im Mikrowellenofen

Summary Decompositions of inorganic and organic materials can be carried out within a few minutes by means of the microwave technique. For dissolving substances with volatile components in the microwave oven, low pressure containers were developed from microwave transparent materials and an excess pressure security system. Results and limitations of the method are explained by examples.