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131.
Simultaneous determination of cobalt,copper, iron and vanadium in crude petroleum oils by HPLC 总被引:1,自引:0,他引:1
Summary A method has been developed for the simultaneous formation and solvent extraction of cobalt (II), copper (II), iron (II) and vanadium (IV) complexes of bis (acetylpivalylmethane)ethylenediamine (H2APM2en) in methyl isobutyl ketone. The complexes are eluted from a reversed phase HPLC column with a mixture of methanol:water:acetonitrile and detection was at 260 nm. The method has been applied to the simultaneous determination of cobalt, copper, iron and vanadium in crude petroleum oils at the ng level. 相似文献
132.
Ja. L. Goldfarb Ju. B. Volkentein L. I. Belenkij 《Angewandte Chemie (International ed. in English)》1968,7(7):519-529
Under normal conditions, thiophene and furan derivatives are substituted in the α position, and no convenient alternative methods for the preparation of β-substitution products have been available until now. The present article describes a method that permits the synthesis of many β-substituted thiophenes and furans. In this method, the carbonyl group in α-aldehydes or ketones of the thiophene and furan series is blocked by complex formation with an excess of aluminum chloride, so that electrophilic substitution takes place in position 4. In another useful method, the carbonyl group is blocked by acetalization. The acetals can be metalated in the ring by organolithium compounds. 相似文献
133.
Pt(II) and Pd(II) dichloride complexes with 5,7-ditertbutyl-1,2,4-triazolo[1,5-a]pyrimidine (dbtp) have been synthesized and characterized by infrared and 1H, 13C NMR, 13C CPMAS spectroscopy. The structures of the cis-PtCl2(dbtp)2 · EtOH (1) and cis-PdCl2(dbtp)(dmso) (2) has been determined by signal-crystal X-ray diffraction. In both complexes the X-ray crystal structures shows that heterocycle ligand (dbtp) binds the central atom monodentate via nitrogen atom N(3). In addition, compound (2) is interesting for its structural features, because it is the first report of mixed dichloride Pd(II) complexes with N-donor (triazolopyrimidine) and S-donor (dimethylsulfoxide) ligands. In this structure the Pd–Cl distances are: 2.302(1) and 2.281(1) Å, Pd–N 2.041(3) Å and Pd–S 2.245(1) Å. The 1H, 13C NMR studies show clearly that these structures are retained in solution. 相似文献
134.
Condensation of 3,5-dinitro-4-chloro-6-methoxy-2-methylquinoline (1) with benzylamine, ethanolamine and/or thioglycolic acid afforded the quinoline derivatives4 a-c. Cyclization of4 a and4 b with alkali and condensation of1 with glycine in sodium carbonate solution furnish 2H-imidazo[4,5-c]quinoline derivatives5 a-c, respectively. Treatment of5 b with benzaldehyde in presence of zinc chloride gave the styryl derivative6. 1 reacted with sodium azide to give the azido derivative4 d, which upon treatment with phenylhydrazine or sodium borohydride yielded the 4-amino derivative4 3. Moreover,1 was treated with phenylhydrazine to give4 f, which cyclized in 10% sodium hydroxide solution to the corresponding v-triazolo[4,5-c]quinoline 3-oxide derivative7. When however4 f was treated with dilute hydrochloric acid, the corresponding phenylpyrazolo[3,4,5-de]quinoline derivative8 was obtained.
Baseninduzierte Cyclisierung einiger Chinoline. Darstellung höherer Stickstoff-Heterocyclen
Zusammenfassung Kondensation von 3,5-Dinitro-4-chlor-6-methoxy-2-methylchinolin (1) mit Benzylamin, Ethanolamin und/oder Thioglycolsäure ergab die Chinolinderivate4 a-c. Cyclisierung von4 a und4 b mit Alkali und Kondensation von1 mit Glycin in Natriumcarbonatlösung lieferte 2H-imidazo[4,5-c]chinolin-Derivate5 a-c. Behandlung von5 b mit Benzaldehyd in Gegenwart von Zinkchlorid ergab das Styrylderivat6. 1 wurde mit Natriumazid zum Azidoderivat4 d umgesetzt, das mit Phenylhydrazin oder Natriumborhydrid zum 4-Aminoderivat4 e weiterreagierte.1 ergab mit Phenylhydrazin4 f, das in 10% NaOH-Lösung zum entsprechenden Triazolo[4,5-c]chinolin-Derivat7 cyclisierte. Aus4 f wurde mit verdünnter Salzsäure das Phenylpyrazolo[3,4,5-de]chinolin8 erhalten.相似文献
135.
《Tetrahedron letters》2004,45(27):5203-5205
The first synthesis of polyfunctionalized 4-ferrocenyl-4H-pyran and 4-ferrocenyl-1,4-dihydropyridine derivatives, as well as some of their relevant properties, including an electrochemical study and some aspects of their biological profile have been described. 相似文献
136.
Starting from the natural neo-clerodane diterpenoid teubotrin (1) several neo-clerodane derivatives (3-7,9-11) have been obtained. The naturally occurring diterpenoid teuscordinon (12) has also been synthesized from teubotrin (1), showing thereby how some of these transformations can be useful for the synthesis of other natural neo-clerodane diterpenes. The latter are of interest due to their activity as insect antifeedants and other important biological properties. 相似文献
137.
Cathodic reduction of -azidocinnamic ester under aprotic conditions on Hg, Pt, or graphite electrodes can be directed to high yields of N,N-diacylated dehydroaminoacid derivates (f.i. addition of acetic anhydride) or to almost quantitative yields of -aminocinnamic ester in very pure form by careful addition of H+-donors. The dehydroamino compounds in turn can be further reduced to the corresponding saturated compounds by following H+-addition and changed electrolysis potential. Almost no dimerization occurs. 相似文献
138.
Hitoshi Shimizu Kazuki Shimizu Atsuko Sugita Tsuyoshi Yamauchi Kazumi Morikawa 《Tetrahedron letters》2004,45(42):7837-7841
Two 21-nor-22-oxa-1α,25-dihydroxyvitamin D3 derivatives have been synthesized in quest of a drug with lower calcemic activity than Maxacalcitol, 22-oxa-1α,25-dihydroxyvitamin D3, being used as antihyperparathyroidism and antipsoriatic drug. Of two 21-nor products obtained, the product carrying one carbon elongated side chain with diethylcarbinol moiety has been found to exhibit comparable differentiation-inducing activity to Maxacalcitol with much lower exhibition of calcemic activity. 相似文献
139.
Yang Jie Wu Shou Quan Huo Li Yang Chen Xia Du 《Journal of organometallic chemistry》1995,490(1-2):249-254
Three series of cyclomercurated ferrocenylimines (2-chloromercurio-ferrocenylimines) have been studied using 13C NMR spectroscopy. Good to excellent linear relationships have been found to exist between the chemical shifts of the carbon atoms in the ferrocenyl moiety and normal Hammett substituent constants σm and σp. The δ values of the iminyl carbon atoms show excellent linear correlations with the σ values. In three series of the ferrocenes, the sensitivity of the carbon atoms to the substituent effect is different, which is discussed in terms of the twist angle between the N-phenyl ring and the C---C=N---C plane. The relative sensitivity of the chemical shifts on different positions in ferrocenyl moiety to the substituent effect has also been presented. 相似文献
140.
Xue Yuan HU Xue Sen FAN Xin Ying ZHANG Gui Rong QU Yan Zhen LI School of Chemical Environmental Sciences Henan Key Laboratory for Environmental Pollution Control Henan Normal University Xinxiang Chongqing University of Medical Sciences Chongqing 《中国化学快报》2005,(7)
Construction of tetrahydropyran rings has attracted a great deal of interests in organic synthesis in recent years1, since tetrahydropyran moiety constitutes a structural unit in a number of natural products2. In addition, tetrahydropyran derivatives possess wide range of biological activities and pharmacological properties, such as anticancer activity3 and antihypersensitivity4. Many methods for the preparation of such compounds have already been developed5. Among them, condensation of α, β… 相似文献