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71.
Abolfazl Olyaei Esmat Chehrehgosha Parashkuhi Saeed Raoufmoghaddam Mahdieh Sadeghpour 《合成通讯》2013,43(24):3609-3617
A series of novel N-heteroaryl α-arylglycines containing naphthol rings has been prepared by one-pot, three-component condensation reaction of glyoxalic acid, heteroaryl amines and naphthols in water at ambient temperature and under reflux conditions in moderate to high yields. The promising advantages such as removal of organic solvent, no need to catalyst, simplicity of the reaction procedure and easy product separation will be discussed in this article. 相似文献
72.
73.
In the presence of 1,8-diazabicycolo[5.4.0]undec-7-ene (DBU) and concentrated H2SO4, 2-naphthol reacted smoothly with α,β-unsaturated trifluoromethyl ketones in CH2Cl2 at room temperature, affording the 3-trifluoromethyl-substituted benzo[f]chromene derivatives in good to excellent yields in a one-pot reaction. [Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resource: Full experimental and spectral details]. 相似文献
74.
A highly efficient protocol has been developed for the three-component reaction of an amine, an aldehyde, and diethyl phopshite catalyzed by ZrOCl2·8H2O, an environmentally friendly catalyst, at ambient temperature. The catalyst exhibited remarkable activity and tolerated a wide variety of functional groups, providing the desired amino phosphonates in excellent yields under solvent-free conditions. Alternatively, the reaction rate can be significantly enhanced by carrying out the reaction in a monomode microwave reactor as a promoter. 相似文献
75.
For the first time, we have observed a combined effect of two bases NaOH/Et3N to promote the diazo transfer reaction of β-oximino esters. This unusual synergistic effect has been employed to obtain α-diazo oxime ethers directly from β-keto esters by one-pot process. This method is simple and cost-effective and the reagents are readily available. 相似文献
76.
New α-cyanoketene-N,S-acetals 2(a–g) and β-dialkylamine-α-cyanoacrylates 3(g–i) were synthesized in good to excellent yields by the reaction of ethyl 2-cyano-3,3-bis(methylthio)acrylate 1 with secondary aliphatic amines (i.e., N-methylalkyl- and N-ethylalkylamines), and pyrrolidine, in the presence of triethylamine, under reflux in ethanol, for 1–16 h, depending on the amine used. Five N-methylalkyl amines and pyrrolidine yielded exclusively mono-substituted N,S-acetals 2(a–f) in good yields. On the other hand, N-ethylbenzylamine gave a mixture of monosubstituted products including N,S-acetal 2g in 35% yield and the unexpected product ethyl 3-[benzyl(ethyl)amino]-2-cyanoacrylate 3g in 50% yield. N-Ethylcyclohexylamine and N-ethylbutylamine did not produce N,S-acetals and gave only the unexpected products ethyl 2-cyano-3-[cyclohexyl(ethyl)amino]acrylate 3h and ethyl 3-[butyl(ethyl)amino]-2-cyanoacrylate 3i in good yields. The α-cyanoketene-N,S-acetals 2(a–f), 2j, and 2k underwent cyclization with the binucleophile hydrazine in ethanol under reflux to afford substituted pyrazoles 4(a–f), 4j, and 4k in good yields. [Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resources: Full experimental and spectral details.] 相似文献
77.
Nádia R. Aguiam Vânia I. CastroAna I.F. Ribeiro Rui D.V. FernandesCarina M. Carvalho Susana P.G. CostaSílvia M.M.A. Pereira-Lima 《Tetrahedron》2013
The multicomponent Ugi reaction is a straightforward method that can be used for the synthesis of highly hindered C-tetrasubstituted amino acids by reacting an amine, a ketone or aldehyde, a carboxylic acid and an isocyanide. In the present work, the synthesis of several α,α-dialkylglycines (α,α-diethylglycine, Deg; α,α-dipropylglycine, Dpg; 1-amino-1-cyclohexanecarboxylic acid, Ac6c) was achieved by solid phase Ugi reaction using resins functionalized with the isocyanide group. Since no resins with these features were available commercially, the functionalization of an aminomethylated resin started by the use of glycine (Gly), β-alanine (β-Ala) and γ-aminobutyric acid (GABA) as spacers. After spacer N-formylation, followed by dehydration, isocyanide functionalised resins were obtained. The resins were then used in solid phase Ugi reaction, using phenylacetic acid as the acid component, 4-methoxybenzylamine as the amine component and different ketones, to afford the desired N-acylated α,α-dialkylglycines in good overall yields (60–80%), after acidolytic cleavage from the resin, thus proving the feasibility of this approach. 相似文献
78.
Latif Kelebekli 《合成通讯》2013,43(22):2998-3009
Stereoselective synthesis of tricyclo[6.2.2.02,7]dodecane-3,6,9,10-tetrol was developed starting from p-benzoquinone. The endo selective Diels–Alder cycloaddition of p-benzoquinone and 1,3-cyclohexadiene afforded the corresponding bicyclic diketone. The synthesis of the title compound was based on the cycloadduct by selective reduction with NaBH4, acetylation with AcCl, and hydroxylation with OsO4-NMO. [Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications® for the following free supplemental resource: Full experimental and spectral details.] 相似文献
79.
K. C. Rajanna N. Maasi Reddy M. Rajender Reddy P. K. Saiprakash 《Journal of Dispersion Science and Technology》2013,34(4):613-616
A Novel Hunsdiecker‐Borodin reaction (HBR) has been carried out efficiently with α,β‐unsaturated aliphatic and aromatic carboxylic acids by using N‐halo succinimides such as N‐chloro succinimide (NCS), N‐bromo succinimide (NBS), and N‐iodo succinimide (NIS) under micellar media. The reaction with α,β‐unsaturated aromatic carboxylic acids afforded β‐halo styrenes in excellent yield while α,β‐unsaturated aliphatic carboxylic acids underwent decarboxylation and to give corresponding halo derivatives. The reactions are dramatically accelerated in micellar media. This procedure works efficiently in CTAB (cetyl trimethyl ammonium bromide), SDS (sodium dodecyl sulfate), and TX (Triton‐X‐100) media under stirred conditions at room temperature. At reflux temperatures the yield of reaction products were further enhanced from good to excellent. 相似文献
80.
Bruce Petrie Ewan J. McAdam Keith H. Richards John N. Lester 《International journal of environmental analytical chemistry》2013,93(13):1343-1355
An ultra-performance liquid chromatography method using a triple quadrupole mass spectrometer was developed and validated for the determination of steroid oestrogens in wastewater matrices. To date, analytical methods established in the literature for 17α-ethinylestradiol have been unable to achieve the proposed predicted no effect concentration of 0.1?ng?l?1. The extensive sample pretreatment and analytical methodology proposed herein enable 17α-ethinylestradiol to be determined at very low background concentrations with a theoretical method detection limit of 0.06?ng?l?1 which has been applied in real environmental matrices. During the validation process, a trickling filter wastewater treatment works was monitored to demonstrate the method's application. Oestrogen removal across the filters demonstrated good removals of natural free oestrogens (≥62.0%) with lower removals of the synthetic oestrogen 17α-ethinylestradiol (29.2%) from wastewaters at 10°C. The method's application illustrates its capability of detecting oestrogen concentrations in real wastewater samples comprising complex organics of comparatively high concentration. Furthermore, a complete process mass balance for 17α-ethinylestradiol is now attainable which has previously posed a challenge owing to the low environmental concentrations typically exhibited, but more significantly as a result of the lower sensitivity inherent in previously reported analytical methods. 相似文献