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1.
M. G. Voronkov A. V. Vlasov N. N. Vlasova 《Russian Journal of Organic Chemistry》2010,46(12):1838-1842
Reactions of acetyl iodide with pyridine at room temperature and with quinoline both at 20–25°C and on cooling to −50°C involve
dehydrohalogenation of acetyl iodide with formation of ketene and pyridinium or quinolinium iodides. The reaction of acetyl
iodide with pyridine at −5 to −50°C led to the formation of N-acetylpyridinium iodide. Benzoyl iodide reacted with both pyridine and quinoline at both −50°C and at 20–25°C to form stable
N-benzoylpyridinium and N-benzoylquinolinium iodides. The reaction of pyrrole with acetyl iodide under analogous conditions was accompanied by polymerization. 相似文献
2.
The Chemical Transport of VO2 with Cl2 and HCl + Cl2 and the Influence of the O2-Coexistence Equilibrium Pressure on the Transport Behaviour The transport behaviour of VO2 with Cl2, HCl, and Cl2 was calculated and compared with the experimental results. VO2 with the upper phase boundary transports with HCl and HCl + Cl2 from the colder to the hotter zone, VO2 of the lower phase boundary does not transport with HCl. The composition of the deposited VO2 is near the upper boundary oxygen richer than in the start space. VO2 does not transport with Cl2. 相似文献
3.
Tsutomu Kagiya Teruho Adachi Kenichi Fukui 《Journal of polymer science. Part A, Polymer chemistry》1969,7(9):2651-2658
The copolymerizations of N-substituted aziridines and cyclic imide were studied. N-Ethylsuccinimide copolymerized with ethylenimine, but N-ethylethylenimine did not copolymerize with succinimide and N-ethylsuccinimide without catalyst. The effect of additives on the copolymerization of ethylenimine with succinimide and that of N-ethylethylenimine with succinimide and N-ethylsuccinimide was also examined. The rate of copolymerization of ethylenimine with succinimide was accelerated by the addition of N-acetylethylenimine or water. The copolymerization of N-ethylethylenimine with succinimide was initiated only by water, but N-ethylethylenimine did not copolymerize with N-ethylsuccinimide in the presence of water. Gas evolved on heating the copolymer of ethylenimine and succinimide was analyzed and confirmed to be ammonia. On the basis of these results the reaction mechanisms of the copolymerization of ethylenimine with succinimide or N-ethylsuccinimide and of N-ethylethylenimine with succinimide initiated by water are discussed. 相似文献
4.
T. I. El-Emary Sh. A. Abdel-Mohsen 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):2459-2474
1,3-diphenyl-1H-pyrazole-4-carboxaldehyde (1) reacted with ethyl cyanoacetate and thiourea to give the pyrimidinethione derivative 2. The reaction of 2 with some alkylating agents gave the corresponding thioethers 3a–e and 7. Thione 2 was cyclized to 5 and 6 upon a reaction with chloroacetic acid and with benzaldehyde, respectively. Thioether 3c was cyclized to 4 upon boiling with sodium acetate in ethanol, and 7 was cyclized to 8 upon boiling in an acetic anhydride-pyridine mixture. The hydrazino derivative 9 was prepared either by boiling 2 and/or 3a with hydrazine. The reaction of 9 with nitrous acid, acetylacetone, triethyl orthoformate, acetic anhydride, and carbon disulfide gave 10–14. The alkylation of 14 with ethyl iodide, phenacyl bromide, and ethyl chloroacetate afforded the alkythiotriazolo pyrimidinone derivatives 15a–c. The dialkyl derivative 16 was produced upon the treatment of 2 with two equivalents of ethyl iodide. Boiling 16 with hydrazine afforded the hydrazino 17. The reaction of 17 with nitrous acid, carbon disulfide, ethyl cyanoacetate, ethyl acetoacetae, and phenacyl bromide gave 18–22, respectively. Some of the newly obtained compounds were tested for their antibacterial and antifungal activities. 相似文献
5.
A. Khodairy H. Abdel-ghany 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):259-273
Abstract 3,4-Diamino-2,5-dicarbethoxythieno(2.3-b)thiophene 1 reacted with malononitrile or ethyl cyanoacetate to afford bis(thienopyrimidin-4-one) derivatives 2a.b The reaction of compound 1 with o-aminothiophenol, o-aminophenol or o-phenylenediamine gave benzothiazolyl-, benzoxazolyl-, benzoimidazolylthienothiophene 3a-c, Chloroacetylation of compound 1 and reacting the resulting compound 4 with malononitrile furnished thienopyrolopyrimidine 6. Fusion of compound 1 with formamide yielded bis(thienopyrimidine) 7 which reacted with POCI3/PCl5 to yield the corresponding chloro derivative 8 which was converted into the corresponding hydrazine derivative 9. Treatment of compound 1 with CS2, NaOH and 1,2 dibromoethane produced the corresponding 1.3 dithiolane 11 which also treated with chloroacetyl chloride or ethyl mercaptoacetate to get the corresponding β-lactame 12 or thiazolidinone 13. On reacting compound 1 with CS2, NaOH and (CH3)2S04 produced the corresponding bi(dithiocarbamate methyl ester) 14 which treated with hydrazine hydrate to yield the corresponding bis(thienopyrimidine) derivative 15. This compound reacted with Lawesson's reagent (LR) to give the desired compounds 16 and 17. While its reaction with (CH3)2 SO4 and NaOH furnished the corresponding methyl derivative 18. Fusion of compound 18 with aniline afforded compound 19. Compound 19 was allowed to react with ethyl acetoacetate, acetylacetone, α-oxoketene dithioacetal, ethoxymethylene malononitrile or LR to get the described compounds 2Oa.b-24 respectively. 相似文献
6.
Heinrich Gruber 《Monatshefte für Chemie / Chemical Monthly》1981,112(6-7):747-758
Chelating resins with thioglycolate anchor groups have been synthesized by reaction of sucrosemethacrylate gels with thioglycolic acid. The capacities of the gels were found to be extremely high for Ag+ (5,3 mmol/g) and Hg2+ (4,9 mmol/g). About 1 mmol Hg2+/g could be recovered from the gel reversibly by treatment with hydrochloric acid. The removal of Hg2+ from aqueous 3M alkalichloride solutions was possible with capacities of 1 mmol/g.Sucrosemethacrylate gels with primary aromatic amino group were reacted with CS2/NH3 to yield gels with dithiocarbamate groups. Gels with thiorea groups were prepared by reaction of the amino groups with NH4SCN/HCl. Diazotation of the amino groups, subsequent reaction with potassium xanthogenate and hydrolysis afforded gels with thiol groups. Thiol containing gels were synthesized also by reaction of the diazotised gels with Na2S2 and subsequent reduction with Na2S. Reaction of the diazotised gels with mercaptans yielded resins with thioether anchor groups. The capacities of the sulfur containing gels were found to be max. 4,1 mmol/g for Hg2+ and 5,9 mmol/g for Ag+. About 35% of the bonded Hg2+ could be eluted resersibly with 3N-HCl. 相似文献
7.
Samuel Natelson 《Microchemical Journal》1982,27(4):466-483
The existence of homoserine lactone in Pisum sativum seedlings is demonstrated. L-Homoserine lactone reacts with hydroxylamine, at neutral or alkaline pH, to form homoserine hydroxamic acid. Procedures are described for preparing L-homoserine lactone and L-homoserine hydroxamic acid. The hydroxamic acid yields a color with maximum absorbance at 492 nm with Fe3+ in 0.25 N HCl. This reaction permitted assay for total homoserine and homoserine lactone. Six-day old Pisum sativum seedlings, with cotyledons removed, were extracted with 90% ethanol. Evaporation of the ethanol and addition of Na2SO4 solution and toluene and centrifugation removed protein lipids and esters. After clarification with activated charcoal, homoserine lactone content was estimated by reaction with NH2OH and Fe3+ reagents. For total homoserine, protein precipitation was with 2 N HCl and toluene. Evaporation to dryness at 60 °C under vacuum converted all homoserine to the lactone. The values found for total homoserine (μmols/g, wet weight) and preformed lactone (%) with the various growth media used were as follows: nitrate 87.4 (14.7%), NH2OH 75.2 (6.3%), water 70.5 (7.9%), urea 56.4 (18.9%). Acetic anhydride added to homoserine hydroxamic acid forms acetohydroxamic acid, which yields a color with maximum absorbance at 505 nm with Fe3+. This color reaction is seven times as sensitive as the reaction of Fe3+ with homoserine hydroxamic acid itself. 相似文献
8.
N-Cyanomethyl and N-propargyl β-amino alcohols are chlorinated with SOCl2 and treated with NaN3 in DMSO. A substitution/cycloaddition process affords in good yields, with high diastereoselectivity and a regioselectivity depending on the substitution pattern of the starting amino alcohol, fused tri- and tetrazoles-piperazines. These heterocycles were further lithiated with n-BuLi at the benzylic position and reacted diastereoselectively with a range of electrophiles. 相似文献
9.
Polycrystalline Fe3 − xVxAl alloys with DO3-type structure and 0 < x < 1.1 were synthesized for the first time and investigated by X-ray, magnetostatic and Mössbauer effect methods. It was found that replacing the iron atoms with vanadium atoms causes disordering of the magnetic structure. In addition to the ferromagnetic phase, a superparamagnetic phase appears and its content increases with increasing vanadium concentration in the alloys. The Curie temperature and the content of ferromagnetic component in the alloys rapidly decrease with x, while the average magnetic moment of the iron atoms in the alloys decreases linearly with x.The alloys with x > 0.5 do not exhibit any long-range magnetic order at temperatures above 4 K. High values of the magnetization and its markedly non-linear variation with the magnetic field intensity together with the absence of Zeeman splitting in the Mössbauer spectra suggest super-paramagnetic properties for these alloys.Mössbauer investigations show that the superparamagnetic relaxation times at room temperature are less than 10−8 s and decrease with increasing x. Considered in conjunction with magnetostatic studies, this appears to indicate a reduction in size of magnetic clusters with increasing x. 相似文献
10.
Andrei Jitianu John Doyle Glenn Amatucci Lisa C. Klein 《Journal of Sol-Gel Science and Technology》2010,53(2):272-279
Hybrid melting gels were prepared by a sol–gel process, starting with a mono-substituted siloxane and a di-substituted siloxane.
Methyl-modified melting gels were prepared using (a) methyltriethoxysilane (MTES) with dimethyldiethoxysilane (DMDES) and
(b) methyltrimethoxysilane (MTMS) together with dimethyldimethoxysilane (DMDMS). The gels with MTES–DMDES were prepared with
concentrations between 50–50 and 75–25 mol%. The gels with MTMS–DMDMS were prepared with concentrations between 50–50 and
70–30 mol%. For both systems, the consolidation temperature, after which the melting gel no longer softens, increased with
an increase in the amount of the mono-substituted siloxane, increasing from 135 to 160 °C for MTES–DMDES and increasing from
145 to 170 °C for MTMS–DMDMS. Coatings formed on mica substrates were about 1 mm thick, and showed no visible cracks. The
surfaces of the coatings were profiled using micro-Raman spectroscopy, which revealed that methyl groups were concentrated
at the surfaces of the films. All contact angles measured with water were greater than 90°. 相似文献
11.
13C Nmr, 1H nmr and ir parameters of coupling products of tetronic acids (4-hydroxy-5H-furan-2-ones) with benzene diazonium sulfate are only consistent with a phenylhydrazone formulation with an almost equal ratio of the syn and anti configurations. These results contrast with those of coupling products of acyclic 3-ketoesters, existing mainly as anti tautomers, and more sharply with the 3-parabromophenylhydrazone of L-dehydro ascorbic acid, which is exclusively syn. 相似文献
12.
B. P. Tarasov V. N. Fokin A. P. Moravskii Yu. M. Shul’ga 《Russian Chemical Bulletin》1997,46(4):649-652
Fullerene hydrides containing 24–26 H atoms per fullerene molecule were obtained by hydrogenation of solid-phase mixtures
of fullerenes with either intermetallic compounds LaNi5, LaNi4.65Mn0.35, CeCo3 or V and Pd metals with gaseous hydrogen at 1.0–2.5 MPa and 573–673 K. These fullerene hydrides decompose at 800 K with evolution
of H2. Upon subsequent heating to 1000 K, vanadium reacts with fullerene to yield a cubic phase of vanadium carbide. The intermetallic
compounds react with fullerene with the formation of a metallic phase of the 3d-metal and destruction of fullerene. Palladium
does not react with fullerene.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 679–683, April, 1997. 相似文献
13.
Reactions of ligands 2-vinylpyridine 1, 4-vinylpyridine 2, 2-allylpyridine 3, 1-allylpyrazole 4, acrylonitrile 5 and allylcyanide 6 with the metallocene derivatives [Mo(η5-C5H5)2H3][PF6] 7, [Mo(η5-C5H5)2HI] 8, [W(η5-C5H5)2H3] [PF6] 9, [Mo(η5-C5H5)2H2] 10, [M(η5-C5H5)2Br2], M = Mo 11, M = W 12 are described. Reaction of 7 with 1, 8 with 1, 3 with 8 and 4 with 8 gave mixtures of metallocyle isomers resulting from coordination of the nitrogen atom to molybdenum followed by internal hydrometallation; reaction of 11 with 1 gave an olefinic π complex; reaction of either 9 or 11 with 1 gave intractable oils; reactions of 8 with 2, 11 with 5, 12 with 5, 11 with 6 and 12 with 6 yielded monosubstituted products in which the ligand is N-coordinated. 相似文献
14.
Donald B. Denney Dorothy Z. Denney Stanley G. Schutzbank 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3):369-372
Abstract The reaction of the isomeric phosphites, 1 and 2, with ozone have been shown to be stereospecific and to proceed with retention of configuration about phosphorus. Similarly ozonization of mixtures of 3 and 4 were found to be stereospecific or very nearly so with retention of configuration about phosphorus. The mechanistic implications of these findings are discussed. Reactions of 1 and 2 with neopentyl and t-butyl hypochlorites proceed in a stereochemically random manner. The formation of a pentacoordinated intermediate is implicated. Reactions of a mixture of 1 and 2 with ethyl thiyl radicals provided phosphorothionates with complete retention of configuration. 相似文献
15.
Virajkumar Gandhi 《Tetrahedron》2010,66(10):1787-14551
Porphyrins with fused pyrene units have been prepared by ‘2+2’ and ‘3+1’ methodologies. Nitration of 1,2,3,6,7,8-tetrahydropyrene, followed by oxidation with DDQ, gave 4-nitropyrene and this condensed with ethyl isocyanoacetate in the presence of DBU or a phosphazene base to generate a pyrenopyrrole ethyl ester. Ester saponification and decarboxylation with KOH in ethylene glycol at 190 °C gave the parent pyreno[4,5-c]pyrrole and this was further condensed with 2 equiv of acetoxymethylpyrroles to afford the corresponding tripyrranes protected at the terminal positions with tert-butyl esters. In a one pot procedure, the ester protective groups were cleaved with TFA and following dilution with dichloromethane, ‘3+1’ condensation with a pyrrole dialdehyde, and dehydrogenation with DDQ, the targeted pyrenoporphyrins were generated in good overall yields. A dialdehyde was also prepared from the pyrenopyrrole intermediate and this reacted to give an opp-dipyrenoporphyrin. The pyrenopyrrole ethyl ester reacted with dimethoxymethane in the presence of an acid catalyst to give a dipyrenopyrrolylmethane, and this was used to prepare an adj-dipyrenoporphyrin using the MacDonald ‘2+2’ approach. The pyrenopyrrole dialdehyde was also used to prepare a porphyrin with fused pyrene and phenanthroline moieties. Although the UV-vis spectra of these new porphyrin systems are unexceptional, pyrenoporphyrins show many of the features necessary for the construction of porphyrin molecular wires. 相似文献
16.
James E. Sealey Charles E. Frazier Gamini Samaranayake Wolfgang G. Glasser 《Journal of Polymer Science.Polymer Physics》2000,38(3):486-494
Esters of cellulose with trifluoroethoxy acetic acid (TFAA) were prepared in homogeneous phase using a mixed anhydride with p‐toluenesulfonic acid. Esters with low degree of substitution (DS), and with DS rising from 0 to 3, had hydrophobic character that prevented the usual association with moisture, which is otherwise typical of cellulose esters with low DS. Cellulose trifluoroethoxy acetate (CT) had Tg's declining by about 40 °C per DS‐unit (from 160 to 41 °C) as DS rose from 1 to 3. Mixed esters, cellulose derivatives with acetate and trifluoroethoxy acetate substituents (CAT), exhibited glass‐to‐rubber and melting transitions by DSC. A linear relationship between both Tg and Tm with respect to DS was recorded with the Tg and Tm separated by 30° to 40 °C. This is consistent with cellulose esters described elsewhere. Surprisingly, the Tg's of CT and CAT were found to be identical when the DS was equivalent to the DS of the fluoro substituents (DSF). © 2000 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 38: 486–494, 2000 相似文献
17.
Chlorine monofluoride reacts with SCl4 and SeCl4 to give the corresponding tetrafluorides, with SeO2 it yields SeOF2 and with excess ClF, SeF4. The behaviour of the tetrafluorides, tetrachlorides, dioxides, and oxydifluorides of sulphur, selenium and tellurium with ClF are compared. 相似文献
18.
E. A. Alekseeva S. S. Basok A. V. Mazepa A. P. Luk’yanenko O. V. Snurnikova A. I. Gren’ 《Russian Journal of General Chemistry》2013,83(9):1738-1743
A series of disubstituted p-tert-butylcalix[4]arenes with N-methoxycarbonylmonoazacrown ether and N-ethoxymonoazacrown ether residues at the lower rim has been prepared via the reaction of di(carboxymethoxy)-p-tert-butylcalix[4]arene with azacrown ethers and subsequent reduction of the resulting amide derivatives. Using UV titration and 1H NMR spectroscopy we have demonstrated the ability of the calixarene with two N-carbonylmonoaza-18-crown-6-ether substituents to form the 1:3 complexes with K+ and Na+ and the 1:2 complexes with Cs+, Sr2+, Cu2+, and Zn2+. The calixarene with two fragments of N-ethoxymonoazo-18-crown ether has formed binuclear complexes with alkali metals cations and mononuclear complexes with transition metals cations. 相似文献
19.
《Analytical letters》2012,45(3):315-321
Abstract A high-performance liquid chromatography assay was developed for the purpose of examining xanthine, hypoxanthine, uridine, thymidine, allopurinol, and oxypurinol in serum of patients with advanced carcinoma treated with methorexate and 5-fluorouracil. After the addition of an internal standard, serum samples were extracted of purines and pyrimidines with trichloroacetic acid and neutralized with tert-amine. Aliquots of the extracted serum were injected onto a C18 reverse-phase column and purines and pyrimidines were eluted with a gradient of MeOH/H2O and KH2PO4 solutions. Absorbance was detected with a variable-wavelength UV spectrophotometer at 254 nm and 280 nm. This assay can be readily applied to quantitate baseline and treatment-induced variations in serum purine and pyrimidine levels which may correlate with clinical response and/or toxicity in patients with cancer. 相似文献
20.
N. M. Bravaya A. N. Panin E. E. Faingol'd O. N. Babkina A. Razavi 《Journal of polymer science. Part A, Polymer chemistry》2010,48(13):2934-2941
We investigated the catalytic performance of both bridged unsubstituted [rac‐EtInd2ZrMe2, rac‐Me2SiInd2ZrMe2] and 2‐substituted [rac‐Et(2‐MeInd)2ZrMe2), rac‐Me2Si(2‐MeInd)2ZrMe2] dimethylbisindenylzirconocenes activated with triisobutyl aluminum (TIBA) as a single activator in (a) homopolymerizations of ethylene and propylene, (b) copolymerization of ethylene with propylene and hexene‐1, and (c) copolymerization of propylene with hexene‐1 (at AlTIBA/Zr = 100‐300 mol/mol). Unsubstituted catalysts were inactive in homopolymerizations of ethylene and propylene and copolymerization of propylene with hexene‐1 but exhibited high activity in copolymerizations of ethylene with propylene and hexene‐1. 2‐Substituted zirconocenes activated with TIBA were active in homopolymerizations of ethylene and propylene and exhibited high activity in copolymerization of ethylene with propylene and hexene‐1, and in copolymerization of propylene with hexene‐1. Comparative microstructural analysis of ethylene‐propylene copolymers prepared over rac‐Me2SiInd2ZrMe2 activated with TIBA or Me2NHPhB(C6F5)4 has shown that the copolymers formed upon activation with TIBA are statistical in nature with some tendency to alternation, whereas those with borate activated system show a tendency to formation of comonomer blocks. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 2934–2941, 2010 相似文献