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991.
Solasodine (I) has been subjected to a number of transformations. The following compounds have been obtained from it by described procedures: 3-acetoxypregna-5,16-dien-20-one (II), 3-acetoxypregn-5-en-20-ol (III), and 3-acetoxypregn-5-en-20-ol (IV). The oxidation of (III) and (IV), the formation of an oxime, and the reduction of the oxime with sodium in ethanol, followed by Hess methylation, has led to 20-dimethylaminopregn-5-en-3-ol (IX) and to 20-dimethylaminopregn-5-en-3-ol (X). From compounds (IX) and (X), by analogy with (III) and (IV) by their oxidation and the preparation of oximes, which were then reduced and methylated, the following were obtained: 3,20-bisdimethylaminopregnane (XVII) and 3,20-bisdimethylaminopregnane (XVIII), and also quaternary salts of the latter.Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 370–374, May–June, 1980. 相似文献
992.
Novel A4B3 Molecules in the System P4Se3–As4Se3 By means of 31P-NMR and masspectroscopic measurements in the system P4Se3–As4Se3 was shown that in the melt and vapour phase at all compositions molecules of the type P4 ? nAsnSe3 are formed. A separation was possible by liquid chromatography (RP 18-column). The concentration distribution of the different species is nearly statistical. In the solid state at ambient temperature regions of solid solubility with α-P4Se3, α+-phase, α-P4S3 and α-As4Se3 structure were observed. P3AsSe3 could be transformed into a plastically-crystalline phase with β-P4S3 structure. At higher temperatures the phase decomposes slowly. The thermal behaviour of PAs3Se3 is strongly influenced by the heating rate. Using low heating rates it decomposes into an amorphous phase, by fast heating a transformation into a metastable plastically-crystalline modification was achieved. During long extraction with CS2 molecules P4 ? nAsnS3 ? mSem are formed by an exchange reaction. They can also be prepared by melting the proper amounts of the elements. 相似文献
993.
A number of novel routes to the alkali metal compounds of hydroquinone M2[p‐C6H4O2] (M = Li, Na, K, Rb, Cs) and M[p‐C6H4O(OH)] (M = K, Rb, Cs) have been synthetically explored. The selective synthesis of the alkali 4‐hydroxyphenolates and 1, 4‐phenylenediolates is based on optimized reaction conditions (solvents, temperatures). All compounds were structurally characterized by means of powder X‐ray diffraction using Rietveld profile refinement including C—C and C—O bond distance restraints. The atomic arrangement of M2[p‐C6H4O2](M = Na, K) (tetragonal, space group: P42/ncm) is characterized by infinite pillars of [M2[3]O2[3]]‐units along the c axis connected by [p‐C6H4O2]2—‐anions with stacking direction along c. The coordinatively unsaturated alkali metals, surrounded by three oxygen atoms, exhibit symmetrical (K) as well as asymmetrical (Na) interactions with the phenylene rings. M[p‐C6H4O(OH] (M = K, Rb) (tetragonal, space group: P4/n) forms hydrogen‐bridged linear chains of [p‐C6H4O(OH)]—‐anions along the c direction. The phenylene planes of neighboring chains have an almost orthogonal arrangement while the interchain planes are parallel. K and Rb are fourfold coordinated by two different oxygen coordination spheres. 相似文献
994.
Ingkaninan K de Best CM van der Heijden R Hofte AJ Karabatak B Irth H Tjaden UR van der Greef J Verpoorte R 《Journal of chromatography. A》2000,872(1-2):61-73
A high-performance liquid chromatography (HPLC) method with on-line coupled ultraviolet (UV), mass spectrometry (MS) and biochemical detection for acetylcholinesterase (AChE) inhibitory activity has been developed. By combining the separation power of HPLC, the high selectivity of biochemical detection, and the ability to provide molecular mass and structural information of MS, AChE inhibitors can be rapidly identified. The biochemical detection was based on a colorimetric method using Ellman's reagent. The detection limit of galanthamine, an AChE inhibitor, in the HPLC-biochemical detection is 0.3 nmol. The three detector lines used, i.e., UV, MS and Vis for the biochemical detection were recorded simultaneously and the delay times of the peaks obtained were found to be consistent. This on-line post-column detection technique can be used for the identification of AChE inhibitors in plant extracts and other complex mixtures such as combinatorial libraries. 相似文献
995.
?zdemir ümmühan Karacan Nurcan ?entürk Ozan Sanlι Sert Sema U?ur Fadime 《Transition Metal Chemistry》2003,28(4):443-446
Five new complexes, [M(CO)5(apmsh)] [M = Cr; (1), Mo; (2), W; (3)], [Re(CO)4Br(apmsh)] (4) and [Mn(CO)3(apmsh)] (5) have been synthesized by the photochemical reaction of metal carbonyls [M(CO)6] (M = Cr, Mo and W), [Re(CO)5Br], and [Mn(CO)3Cp] with 2-hydroxyacetophenone methanesulfonylhydrazone (apmsh). The complexes have been characterized by elemental analysis, mass spectrometry, f.t.-i.r. and 1H spectroscopy. Spectroscopic studies show that apmsh behaves as a monodentate ligand coordinating via the imine N donor atom in [M(CO)5(apmsh)] (1–4) and as a tridentate ligand in (5). 相似文献
996.
Pál Tapolcsányi Bert U.W Maes Katrien MonsieursGuy L.F Lemière Zsuzsanna RiedlGyörgy Hajós Bart Van den DriesscheRoger A Dommisse Péter Mátyus 《Tetrahedron》2003,59(31):5919-5926
Palladium-catalyzed intramolecular arylation of 2-benzyl-5-(2-bromophenyl)-4-phenylpyridazin-3(2H)-one yielded hitherto unknown 2-benzyldibenzo[f,h]phthalazin-1(2H)-one. The synthesis of this new tetracyclic pyridazinone from 2-benzyl-5-(2-aminophenyl)-4-phenylpyridazin-3(2H)-one via a Pschorr type reaction was also investigated. Similarly, the construction of 2-methyldibenzo[f,h]cinnolin-3(2H)-one from 2-methyl-5-(2-bromophenyl)-6-phenylpyridazin-3(2H)-one and 2-methyl-5-(2-aminophenyl)-6-phenylpyridazin-3(2H)-one is also reported. Removal of the N-benzyl protective group of 2-benzyl-dibenzo[f,h]phthalazin-1(2H)-one with AlCl3 yielded unsubstituted dibenzo[f,h]phthalazin-1(2H)-one. 相似文献
997.
Tetrafluoroaurates(III) of Lanthanoides M2F[AuF4]5 (M = Tb, Dy, Ho, Er) Tetrafluoroaurates(III) M2F[AuF4]5 with M = Tb, Dy, Ho, Er, all yellow, have been obtained. From single crystal data they crystallize triclinic, space group P1 -C1i (No. 2) with Tb: a = 1 194,34(7) pm, b = 798,46(6) pm, c = 902,02(7) pm, α = 89,033(7)°, β = 88,990(6)°, γ = 89,006(7)°; Dy: a = 1 191,66(9) pm, b = 796,33(8) pm, c = 899,65(9) pm, α = 88,956(8)°, β = 89,056(8)°, γ = 88,972(8)°; Ho: a = 1 189,06(10) pm, b = 795,46(6) pm, c = 896,81(7) pm, α = 88,912(8)°, β = 89,101(7)°, γ = 88,873(8)°; Er: a = 1 185,20(40), b = 793,98(14), c = 893,83(20), α = 88,751(23)°, β = 89,187(26)°, γ = 88,884(9)° 相似文献
998.
Structural analysis of underivatized sialic acids by combined high-performance liquid chromatography-mass spectrometry 总被引:1,自引:0,他引:1
A K Shukla R Schauer U Schade H Moll E T Rietschel 《Journal of chromatography. A》1985,337(2):231-238
Mass spectra of chemically ionized, positive ions of underivatized N,O-acylated sialic acids, 2-deoxy-2,3-didehydro-N-acetylneuraminic acid and sialyl-alpha(2-3)-lactose were obtained by combined high-performance liquid chromatography--mass spectrometry, using a direct liquid inlet system. The mass spectra of the different compounds for which fragmentation schemes are proposed enable the differentiation between sialic acids, although the localization of O-substituents is not possible. However, since the various sialic acids separated well on high-performance liquid chromatography, combined high-performance liquid chromatography-mass spectrometry allowed their unequivocal characterization. 相似文献
999.
M. Akram N. U. Khattak A. A. Qureshi Arshid Iqbal K. Ullah I. E. Qureshi 《Journal of Radioanalytical and Nuclear Chemistry》2004,261(2):429-435
Neutron induced radiography has been applied to the determination of boron concentrations in drinking water, collected from natural springs of Reshian and Muzaffarabad areas of Azad Kashmir, Pakistan, using CR-39 etched track detectors. The technique is based upon the simultaneous irradiation with thermal neutrons of a sample of unknown concentration and a standard of known boron concentration, fixed on a track detector. The subsequent counting of alpha and 7Li tracks in the detector resulting from the 10B(n,)7Li nuclear reaction is done after chemical etching. Boron concentration in the sample is determined by comparing 7Li and alpha-particle track density with that of a standard of known boron concentration. Boron concentrations in drinking water samples from Muzaffarabad and Reshian area of Azad Kashmir have been found to vary from (0.054±0.001) mg/l to (0.250±0.004) mg/l with an average of (0.16±0.002) mg/l. The observed concentration of boron in drinking water has been found to be less than the provisional Maximum Acceptable Concentration level (0.4 mg//l) of WHO. The drinking water from the reported area has been found to be within safe limits as far as boron related health hazards are concerned.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
1000.