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1.
The Diels–Alder reactions of three β-chloro-α,β-unsaturated carbonyl compounds 1–3 with different dienes were carried out to afford highly functionalized cyclohexenes 4–9, bearing quaternary centers, in good yields. These cycloadducts (CAs) undergo dehydrochlorination with subsequent aromatization in the presence of 1,8-diazabicyclo[5.4.0]undec-7-ene DBU to produce new substituted benzenes 11–14. Compound 10 is the product of lactonization and removal of an HCl molecule from compound 7. All products were characterized by NMR, IR, elementary analysis and some of them by MS. Structure assignments of isomers were carried out on the basis of NMR chemical shifts and coupling constants using 1D, 2D and heteronOe NMR techniques. 相似文献
2.
O. A. Luk’yanov G. A. Smirnov P. B. Gordeev 《Russian Journal of Organic Chemistry》2007,43(8):1228-1231
A preparation method was developed for previously unknown tetrazole derivatives containing in the 1, 2, and/or 5 positions of the tetrazole ring N-methyldiazene-N-oxide-N′-oxymethyl groups. 相似文献
3.
β-Methoxycarbonyl-γ-butyrolactones bearing a γ-aromatic substituent were prepared via copper-catalyzed reductive aldol addition/lactonization domino reactions of ketones with α,β-unsaturated dicarboxylate esters and a silane under ambient temperature. The reaction has advantage of using readily available reagents, mild conditions and high efficiency. 相似文献
4.
A. A. Shamitov I. K. Garkushin A. V. Kolyado E. P. Petrov 《Russian Journal of Physical Chemistry A, Focus on Chemistry》2018,92(2):300-303
The n-decane–n-hexadecane–cyclododecane, n-decane–cyclododecane, and n-hexadecane–cyclododecane systems are studied by means of low-temperature differential thermal analysis using a differential scanning heat flow calorimeter. It is noted that all studied systems belong to the eutectic type. It is concluded that in the n-decane–n-hexadecane–cyclododecane system, the eutectic composition contains 85.0 wt % n-С10Н22, 4.0 wt % n-С16Н34, and 11.0 wt % С12Н24. It has a melting point of ?35.0°C. 相似文献
5.
6.
Rottava I Cortina PF Martello E Cansian RL Toniazzo G Antunes OA Oestreicher EG Treichel H de Oliveira D 《Applied biochemistry and biotechnology》2011,164(4):514-523
The main objective of this work is to present the optimization of the biotransformation of R-(+)-limonene and (−)-β-pinene aiming at the production of α-terpineol by strains of fungal and yeasts previously isolated
by our research group using the methodology of experimental design. New optimized experimental data on α-terpineol production
by the biotransformation of R-(+)-limonene and (−)-β-pinene using newly isolated microorganisms are reported in this work. Conversion of about 1,700 mg/L
was achieved when R-(+)-limonene was used as substrate and the newly isolated strain 05.01.35 as microorganism at the central point of the experimental
design, corresponding to a substrate concentration of 1.75%, mass of inoculum of 2 g, and substrate to ethanol volume ratio
of 1:1. The same experimental condition led to higher conversions when (−)-β-pinene was used as substrates and the strains
coded as 04.05.08 and 01.04.03 as microorganism. Here, conversions of about 770 mg/L were achieved. 相似文献
7.
Summary.
N-Acyl--hydroxyglycinates were transformed into N-acyl--triphenylphosphonioglycinates by (i) phosphorylation with Ph
3PBr2 in the presence of Et
3N or (ii) in reaction with DCC and Ph
3P·HBF4 in the presence of catalytic amounts of Ph
3P as well as (iii) by a new kind of Mitsunobu reaction with Ph
3P·HBF4 as a nucleophile conjugated acid. The N-acyl--triphenylphosphonioglycinates can be effectively used without isolation for a nucleophilic displacement of the triphenylphosphonium group to obtain corresponding -substituted -amino acid derivatives. 相似文献
8.
Yasunori Matsui Minoru Shigemori Toshiyuki Endo Takuya Ogaki Eisuke Ohta Kazuhiko Mizuno Hiroyoshi Naito Hiroshi Ikeda 《Research on Chemical Intermediates》2018,44(8):4765-4774
The semiconductor properties of the earliest known stable radical, α,γ-bisdiphenylene-β-phenylallyl radical (Koelsch radical, 1?) were assessed using spectroscopic and electrical techniques. This radical undergoes reversible redox processes, and it has low redox potentials. In addition, 1? possesses long wavelength absorption bands, owing to the existence of a singly-occupied molecular orbital whose energy level lies between those of the HOMO and LUMO. A spin-coated thin-film of 1? displays photocurrent and an electron mobility of 6.3 × 10?7 cm2 V?1 s?1 on a trially-fabricated organic field effect transistor. 相似文献
9.
The sodium salt of N-(6-chloronicotinoyl)-γ-aminobutyric acid, a structural analog of the known nootropic and vasidilating drug picamilon, was synthesized via Schotten–Baumann
acylation of γ-aminobutyric acid with 6-chloronicotinoyl chloride and subsequent neutralization of the N-(6-chloronicotinoyl)-γ-aminobutyric acid that was obtained in >60% yield. 相似文献
10.
D. T. Souza A. S. R. Bispo E. P. S. Bon R. R. R. Coelho R. P. Nascimento 《Applied biochemistry and biotechnology》2012,166(6):1575-1585
In the present paper, endo-β-1,4-xylanase production by Aspergillus fumigatus was evaluated in solid-state fermentation using low-cost substrates such as sugarcane bagasse (SCB), brewer’s spent grain
(BSG), and wheat bran (WB). The partial characterization of the crude enzyme was also performed. In the experimental conditions,
the highest levels of endo-β-1,4-xylanase production by A. fumigatus FBSPE-05 occurred within 8 days incubation when using SCB/liquid medium at 1:2 ratio (219.5 U g−1) and 4 days incubation when using WB/liquid medium at 1:1 ratio (215.6 U g−1). Crude enzyme from this last condition was used to enzyme characterization, showing best enzyme activity at 60 °C and pH 6.0,
which suggests a thermophilic endoxylanase. The crude enzyme retained 73% of its activity after 1 h at 60 °C, and zymogram
has shown three bands of endo-β-1,4-xylanase activity, with different molecular masses. A. fumigatus FBSPE-05 was able to grow and produce good levels of endo-β-1,4-xylanase using agro-industrial by-products, making this strain
worthy for further investigation. To our knowledge, this is the first study reporting the use of SCB and/or BSG as sole substrates
for endoxylanase production by solid-state fermentation using A. fumigatus. 相似文献
11.
20S-Protopanaxadiol (3β,12β,20S-trihydroxydammar-24-ene) 3-, 12-, and 20-O-β-D-galactopyranosides were synthesized for the first time. Condensation of 12β-acetoxy-3β,20S-dihydroxydammar-24-ene (1) and 2,3,4,6-tetra-O-acetyl-α-D-galactopyranosylbromide (α-acetobromogalactose) (2) under Koenigs–Knorr conditions with subsequent removal of the protecting groups resulted in regio- and stereoselective formation
of 20S-protopanaxadiol 3-O-β-D-galactopyranoside, an analog of the natural ginsenoside Rh2. Glycosylation of 12β,20S-dihydroxydammar-24-en-3-one (5) by 2 with subsequent treatment of the reaction products with NaBH4 in isopropanol and deacetylation with NaOMe gave 20S-protopanaxadiol 12- and 20-O-β-Dgalactopyranosides. 相似文献
12.
V.?R.?Akhmetova E.?M.?Bikbulatova N.?S.?Akhmadiev V.?M.?Yanybin T.?F.?Boiko R.?V.?Kunakova A.?G.?Ibragimov
Catalytic aminomethylation of pyrrole and indole with N,N,N′,N′-tetramethylmethanediamine in the presence of 5 mol % of ZrOCl2·8H2O proceeds selectively at the positions 2, 5 of pyrrole and 1, 3 of indole. Carbazole under the same conditions affords 3-formyl-9-aminomethyl derivative. The reaction in the presence of 5 mol % of K2CO3 occurs as monoaminomethylation: for pyrrole at the position 2, for indole at the position 3, and for carbazole at the nitrogen atom of the substrate. Water-soluble 1,1′-(1H-pyrrole-2,5-diyl)bis(N,N-dimethylmethanamine) exhibits a fungistatic activity with respect to phytopathogenic fungi Rhizoctonia solani. 相似文献
13.
Bohumil Proksa Richard Hercek Tibor Liptaj Nada Prónayová 《Monatshefte für Chemie / Chemical Monthly》2009,140(5):485-487
Abstract A new compound was isolated from the reaction mixture after O-demethylation of 6-O-acetyl-10α-acetoxycodeine with boron tribromide. The structure of this compound, 10α-hydroxy-β-isomorphine, was elucidated by spectral data, and its spatial arrangement was deduced from an NOE experiment. Capillary zone
electrophoresis was used for separation of morphine and its 10-hydroxy analogues.
Graphical abstract
相似文献
14.
Amanda L. Santos Gilberto O. Chierice Kenneth S. Alexander Alan Riga Ellen Matthews 《Journal of Thermal Analysis and Calorimetry》2009,96(3):821-825
Eugenol is the main volatile compound extracted oil from clove bud, Syzygium aromaticum L., and used in traditional medicine, as a bactericide, fungicide, anesthetic, and others. Its extraction was performed using
hydrodistillation which is the most common extraction technique. Its components and thermal behavior were evaluated using
gas chromatography (GC) and differential scanning calorimetry (DSC), which provide a better characterization of these natural
compounds. This extracted product was compared to the standard eugenol results. The GC results suggested ~90% eugenol was
found in the total extracted oil, and some of its boiling characteristics were 270.1 °C for peak temperature and 244.1 J g−1 for the enthalpy variation.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
15.
O. B. Kazakova E. F. Khusnutdinova A. N. Lobov N. I. Medvedeva L. V. Spirikhin 《Chemistry of Natural Compounds》2011,47(4):579-582
Allylic oxidation of 19β,28-epoxy-A-neo-5β-methyl-25-nor-18α-olean-9-ene by ozone produced 19β,28-epoxy-A-neo-5β-methyl-25-nor-18α-olean-9-en-1-one. 相似文献
16.
17.
Guo T Geis S Hedman C Arndt M Krick W Sonzogni W 《Journal of the American Society for Mass Spectrometry》2007,18(5):817-825
Beta-methylamino-L-alanine (BMAA) is a neurotoxic amino acid that can be produced by cyanobacteria in aqueous environments. To analyze this compound by gas chromatography/mass spectrometry (GC/MS), BMAA must be derivatized to a nonpolar, volatile compound. This can be accomplished by reacting BMAA with ethyl chloroformate. While carrying out electron ionization (EI) mass spectrometric analysis on the (13)C-labeled derivative, it was discovered that the formation of an ion with a peak at m/z 245.12 is the result of [CH(3)CH(2)O.] loss from the amino groups resulting from alpha-cleavage. This differs from previous reports that attributed this peak to alpha-cleavage of the carboxylic ester portion of the BMAA derivative. This finding is important for understanding BMAA derivative mass spectrometric fragmentation patterns and ultimately to properly identifying and quantifying BMAA. Fragmentation pathways for the formation of other major peaks observed in the EI mass spectra are also proposed. 相似文献
18.
Aruna P. Maharolkar A. G. Murugkar P. W. Khirade S. C. Mehrotra 《Russian Journal of Physical Chemistry A, Focus on Chemistry》2017,91(9):1710-1716
The refraction, dielectric, viscosity, density, data of the binary mixtures of N,N-dimethylacetamide (DMA) with n-butanol at 308.15 and 313.15 K. The measured parameters used to obtain derived properties like Bruggeman factor, molar refraction and excess static dielectric constant, excess inverse relaxation time, excess molar volume and excess viscosity, excess molar refraction. The variation in magnitude with composition and temperature of these quantities has been used to discuss the type, strength and nature of binary interactions. Results confirm that there are strong hydrogen-bond interactions between unlike molecules of DMA+ n-butanol mixtures and that 1: 1 complexes are formed and strength of intermolecular interaction increases with temperature. 相似文献
19.
Using the eutectic-type T–x–y diagram as an example, it can be represented the analysis of its geometrical construction dependence on the temperature of
a component two polymorphous modifications which participate in mono- and invariant metatectic and invariant eutectic (eutectoid)
transformations above or below (and within) binary eutectics temperature intervals and below a ternary eutectic temperature.
Computer models for considered phase diagrams have been designed. Such models help to solve applied tasks like visualization,
isopleths and isothermal sections decoding, mass balances calculation and evaluation of phase and conglomerate concentration
in microstructure. 相似文献
20.
N. V. Kovganko S. N. Sokolov Yu. G. Chernov Zh. N. Kashkan V. L. Survilo 《Chemistry of Natural Compounds》2010,46(5):750-755
New derivatives of steroidal 6-ketoximes containing α-chloropyridine neonicotinoid groups characteristic of bioactive compounds were synthesized by formation of oximes of cholestane
and stigmastane 3β,5-dihydroxy-6-ketosteroids with O-(2-chloropyridin-5-ylmethyl)hydroxylamine in the presence of zinc or tin(IV) chloride. 相似文献