A Simple and Efficient Procedure for the Preparation of O-aryl-O-ethyl-S-allyl Thiolophosphates

HubeiNaturalScienceFoundationforfinancialsupportChap-cyethy-S-allylthiOlwioSPhates(2a-j)havePOtenhalbiologicalachvihes.Inl983,Y.TamaruandZYoshidarePOrtedPallatuxn(o)catalyZedthiono-ffooloallylicrearr~mentOfcrallylphoSPhoro-andphoSPhonotheonaes,andaiSOreinvestigaedthennalrearrangementOfa-andy-methallyldiethyphOSPhorothionaesinrelallontotheregioselectivityObserVedinthePalladium(O)catalySisl'].InourPreviousStUdy,Hg(II)catalghcandthermalffoono-ffoolorearrangmentOfcrPrOPargylcreqlp…     

A Green Synthesis of 2-Ethylanthraquinone by Dehydration of 2-(4''''-ethylbenzoyl) benzoic Acid over Solid Acid Catalysts

2-EAQ is an important intermediate for the synthesis of hydrogen peroxide, pharmaceu- ticals, pesticides, and dyes. With the increasing demand for hydrogen peroxide, it needs to enhance the yields of 2-EAQ. However, in the conventional process, concentrated H2SO41-2 is employed as the catalyst in the dehydration of BE acid for the synthesis of 2-EAQ, which produces a series of environmental impacts and safety concerns. For these reasons, a substitute process, which has little or no hazard…     

A Simple and Efficient New Approach to the Total Synthesis of (±)-4-Amino-3-(4-Chlorophenyl)-Butyric Acid (BACLOFEN)

Based on the utilization of a [2+2] cycloaddition reaction between dichloroketene and an appropriated olefin as a key step, we describe a new and simple four step approach to the total synthesis of (±)-4-amino-3-(4-chlorophenyl)-butyric acid (BACLOFEN), a selective GABA_B agonist used as antispastic agent     

A Convenient Procedure for Preparation of 1-(1-Aminoalkyl)-1-cyclopropanols from N-Benzyl α-Amino Acid Esters

The reaction of N-benzyl -amino acid ethyl esters with ethylmagnesium bromide in the presence of a catalytic amount of titanium tetraisopropoxide leads to formation of the corresponding 1-aminoalkyl- 1-cyclopropanols in high yields. Hydrogenation of the latter over palladium catalyst ensures selective removal of one or two protecting benzyl groups from the nitrogen atom.     

A Simple Method for the Preparation of ZnO Prickly Spheres

The synthesis of ZnO prickly spheres using precipitation followed by heating treatment was investigated. Zn(OH)2 precursor was prepared by precipitation process using Zn(CH3COO)2-2H2O in mixed 1-propanol-water solvent. Sodium dodecyl sulfate (SDS) as the anionic surfactant was added to control the morphology. The size and structure of ZnO prickly spheres were studied using XRD, TEM and SEM. The results showed that the morphologies and size of the spheres strongly depended on the volume ratio of 1-propanol /water and molar ratio of SDS/Zn2+. ZnO prickly spheres composed of nanorods could be obtained, when the volume ratio of 1-propanol/water = 2:3 and the molar ratio of Zn2/SDS= 450:1.     

A Facile Synthesis of (±)2-(4-Chlorophenyl)-α-Methyl-5-Benzoxazoleacetic Acid (Benoxaprofen)

A convenient four step procedure for the synthesis of benoxaprofen is described starting with 4-hydroxyphenylacetic acid.     

Stability of Mefenamic Acid in the Inclusion Complex with β-Cyclodextrin in the Solid Phase

The inclusion complex of mefenamic acid with -cyclodextrin was obtained by the method of coprecipitation from diethyl ether. The product was identified by the thermogravimetric and X-ray methods. The complex stability constants were determined by the potentiometric method. The effect of -CD on the solubility and stability of mefenamic acid was analysed.     

Fiber-in-Tube Solid Phase Extraction (FIT-SPE) for Miniaturized Sample Preparation Process

A typical analytical separation procedure has several important steps: sample preparation, isolation, identification, quantitation, statistical evaluation and final decision. Each step is alwayscritical to obtain correct results to fulfill the analytical purpose. In these various steps sample     

Silica Sulfuric Acid,an Efficient and Recyclable Solid Acid Catalyst for the Synthesis of 4,4′-(Arylmethylene)bis (1H-pyrazol-5-ols)

Silica sulfuric acid (SSA) is employed as a recyclable catalyst for the condensation reaction of aromatic aldehydes with 3-methyl-l-phenyl-5-pyrazolone. This condensation reaction is performed in a mixture (1:1 v/v) of water–ethanol at 70 °C, giving 4,4′-alkylmethylene-bis(3-methyl-5-pyrazolones) in 75–93% yields.

Fiber-in-Tube Solid Phase Extraction (FIT-SPE) for Miniaturized Sample Preparation Process

Atypicalanalyticalseparation procedurehasseveralimportantsteps :samplepreparation ,isola tion ,identification ,quantitation ,statisticalevalua tionandfinaldecision .Eachstepisalwayscriticaltoobtaincorrectresultstofulfilltheanalyticalpur pose .Inthesevario…     

Synthesis of 2-Methoxy-4-(methylsulfanyl)benzoic Acid — An Intermediate Product in the Preparation of the Cardiotonic Drugs Sulmazole and Isomazole

Russian Journal of Organic Chemistry - Readily available 4-methyl-3-nitrobenzenesulfonic acid and 2-methyl-5-nitrophenol were used to develop two alternative approaches to the synthesis of...     

A Convenient Procedure for the Synthesis of 6-O-Mono-Phosphate β-Cyclodextrins

Abstract

The synthesis of β-cyclodextrin derivatives bearing one phosphate group on the primary rim is reported. These compounds were prepared in good to excellent yields, by reacting β-cyclodextrin with dialkyl chlorophosphates in the presence of 4-dimethyl amino pyridine (DMAP) catalyst and dimethylformamide (DMF) as solvent. The methodology described is highly selective and the purification of the title compounds is simple, because difficulties due to phosphate regioisomers mixture are avoided.     

Synthesis of (4R)-α-Terpineol

Thesynthesisofopticallyactivecompoundsisanimportantissueinmodemorgan-icchendstry-7-Terpineol,anaturalproductisolatedfrompetitgrainoil,longleafpineoi1andcaeputoill'J,hasbeenasynthetictargetduringthecourseofourstudiesontheasymmetriccatalisedDiels-AlderreactionlvInthispaper,l-phenylsulfOnyl-3-buten-2-one(l)wasusedasthesulfOnyl-functionalizedche1atingenoneforthesynthesischiral2-Terpineol(5)byaasymmetriccata1isedDiels-Alderreaction.TherouteforthesynthesisofopticallyaCtivea-Terpineo1(5)isshownin…     

Xanthan Sulfuric Acid: An Efficient,Biosupported, and Recyclable Solid Acid Catalyst for the Synthesis of 4,4′-(Arylmethylene)bis(1H-pyrazol-5-ols)

A simple and efficient method has been developed for the synthesis of 4,4′-(arylmethylene)bis(1H-pyrazol-5-ols) by the condensation reaction between substituted aldehydes, and 1-phenyl-3-methylpyrazol-5-one in the presence of xanthan sulfuric acid (XSA) as a solid acid catalyst. This method is simple and cost-effective with short reaction times. Yields are excellent with high purity, and the catalyst could be easily recycled.     

Phosphomolybdic Acid: An Efficient and Recyclable Solid Acid Catalyst for the Synthesis of 4,4′-(Arylmethylene)bis(1H-pyrazol-5-ols)

An efficient and environmentally friendly method has been developed for synthesis of 4,4′-(arylmethylene)bis(1H-pyrazol-5-ols) by condensation reaction of aromatic aldehydes with 3-methyl-l-phenyl-5-pyrazolone in the presence of phosphomolybdic acid as a recyclable catalyst in ethanol at ambient temperature in excellent yields.     

Total Synthesis of (-)-Baimuxifuranic Acid

ThenatieChenmanginclha,oneofthemoStbeandexpensivCherbaldrugSin~tionalChjnsemdednesisthewoodypartofAquIIarasinensisW.)Gilg.,whoseVofatileoilseforitaIUUnberofinterestinbiologicalandphannacologicalactivities,suchasanestheha,muscularrelaxationandanalgesta'.ReCentiyYanetaI2isolated(-)taim~cacid(1)frOmtheVOboleoilofChenAlang,anddeennineditSStIUCtUrbySpeCtrscoPicmethodandred~1toaknowncornPOunisobaimndnolCoInPOun1isthefirStcarboxylicacidwithdihydragarohanskeletonisolatedfromnisources.He…     

Note on the Preparation of L-α,γ-Diaminobutyric Acid

In our laboratory we needed L-α,γ-diaminobutyric acid and we successfully tried to improve the method of Adamson (1) (scheme 1). As there are many articles in the literature dealing with the synthesis of this compound (sometimes making use of tedious isolation procedures and leading to yields ranging from 15 to 62% (2–8)), it appeared useful to describe our method.     

A Facile Procedure for the oxidative Coupling of 2-Naphthol and 2-Naphthalenethiol in Solid State

l,lLBi-2-naPhtholshavebeenwidelyappliedasimportantchiralauxiliariesandligands..tinorganicchemistry'.TheconversionofthiolstothecorrespondingdisulphidesisofintCrestbothfromabiological'andpracticalpointofview.ForthesynthesisofbinaPhtholsanddisulphides,theoxidativecouplingofnaphtholsandthiolshaslongbeenarecognisedmethodofchoice.Variousoxidantscanbringaboutthecouplingofnaphthols'andthiols4insolution,buttheyoftenleadtolowyieldsorsufferfromdisadvantagesduetotheinsolubilityofoxidant,naPhthoIandthiol…     

Synthesis of 3(R)-(t-Butyldiphenylsilyloxy)-1-penten-4-yne, via an Improved Procedure for Aldehyde-to-Alkyne Homologation

InourstudyonthetotalsynthesisofnaturalbioactivepolyacetyIenesisolatedfromCallusofPanaxginseng',weneededtopreparethefragmentofhydroxyprotected3(R)-hydroxy-l-penten-4-yne(1).Alkynesareusefulintermediatesinorganicsynthesis,andoneofthemostconvenientmethodsofpreparingalkynesistheone-carbonhomologationorginallydevelopedbyMckelvieetal2.,andwhichwaslaterextendedbyCoreyandFuchs3.Thisprocedurereqiurestheformationofal,l-dibromoalkenebytheadditionofdibromomethylenetriphenylphosphoranetoanaldehyde.Theal…