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91.
Zbigniew GrobelnyAndrzej Stolarzewicz Barbara Morejko-Bu?Adalbert Maercker 《Journal of organometallic chemistry》2002,660(1):6-13
The linear ether bond was exclusively cleaved in benzyl glycidyl ether and triphenylmethyl glycidyl ether under the influence of K−, K+(15-crown-5)2 (1), whereas the strongly strained three-membered oxacyclic ring remained undisturbed. Potassium glycidoxide and benzylpotassium were found as the primary reaction products of benzyl glycidyl ether with 1. Subsequently, benzylpotassium reacted with benzyl glycidyl ether giving the next potassium glycidoxide molecule and bibenzyl. Benzyl phenyl ether was used as a model compound to explain the mechanism of bibenzyl formation. The reaction of triphenylmethyl glycidyl ether with 1 resulted in potassium glycidoxide and stable triphenylmethylpotassium. After treating with a quenching agent a new glycidyl ether or glycidyl ester was obtained from potassium glycidoxide. These results were found when the reaction occurred at the excess of glycidyl ether. In another case, i.e. at the excess of 1 further reactions took place with the participation of potassium anions and various new compounds were observed in the reaction mixture after benzylation or methylation. Thus, the method of substrates delivery influences the course of studied processes in a decisive way. 相似文献
92.
A series of crown ethers with single benzene, naphthalene, biphenyl and binaphthyl units are prepared by the intramolecular Okahara cyclization of appropriate symmetrical diols. The method is used to synthesize new crown ether compounds and to prepare previously-reported crown ethers in improved yields. 相似文献
93.
Zusammenfassung Die Bestimmungsmethode für Mikromengen elementaren, in Sulfiden enthaltenen Schwefels mit Natriumazid und Jod wurde modifiziert. Der Analyse geht die Aufspaltung des S8-Ringes voraus, die man dank der nukleophilen Wirkung von N3
– in DMF-Lösung erreicht. Diese Methode wurde auf die Bestimmung des Schwefels in Indium-, Blei-, Antimon- und Wismutsulfid angewandt. Sie ist einfach und empfindlich. Ihre Fehlergrenze liegt bei ± 4%.
Determination of microamounts of sulfur after cleavage of the S8 king in indium, lead, antimony and bismuth sulfides by means of an induced reaction of sodium azide with iodine
Summary The determination of microamounts of elemental sulfur contained in sulfides using sodium azide and iodine was modified. The analysis was preceded by cleavage of the S8 ring, which is achieved by virtue of the nucleophilic action of N3 – in DMF solution. This method was applied to the determination of sulfur in indium, lead, antimony and bismuth sulfides. It is simple and sensitive. Its limit of error is ±4%.相似文献
94.
Bronislaw Czech 《Tetrahedron letters》1980,21(43):4197-4198
Components for polymer-supported catalysts, hydroxymethyl-substituted 15-crown-5 and 18-crown-6 were prepared from readily available starting materials on relatively simple way. 相似文献
95.
Zusammenfassung Die Bestimmung von Wolfram im kapazitiv gekoppelten Mikrowellenplasma (CMP) wurde untersucht. In unserem N2-Plasma beträgt die kinetische Gastemperatur 4450 K, die Anregungstemperatur bis zu 5590 K. Die relativen Intensitäten von 45 Atomlinien des Wolframs im Bereich 450 bis 185 nm werden angegeben. Ionenlinien sind nicht zu beobachten. Analytisch am besten geeignet ist die Linie WI 400,875 nm. Mit ihr sind in wäßriger Lösung 1,5 ppm W nachweisbar, in Gegenwart von 0,01 M Na+ noch 5 ppm. Neben viel Ti ist die Linie WI 407,436 nm vorzuziehen. — Die Wirkungen und Wechselwirkungen von Alkaligehalt, Generatorleistung, Beobachtungshöhe und Zerstäuberdruck auf die Linienintensität wurden mit einem Faktorenversuchsplan untersucht und ihre optimale Einstellung nach dem Simplexverfahren ermittelt. — In Stählen und anderen Legierungen wurden 0,2–80 % W bestimmt.Wir danken der Deutschen Forschungsgemeinschaft für die Gewährung von Sachbeihilfen, den Herren M. Brühl-Saager, U. Tracht und E. Antfang für ihre Mithilfe und Herrn Prof. F. Umland für die Förderung unserer Arbeiten. 相似文献
96.
Marek L. Główka Zbigniew J. Kamiński Gastone Gilli Valerio Bertolasi 《Journal of chemical crystallography》1986,16(4):569-576
C14H17NO4 crystallizes in the monoclinic space groupP21/n (Z=4) witha=10.208(2),b=10.888(2),c=11.909(2) Å, and=90.89(2)°. The structure was solved by direct methods and refined by full-matrix LSQ to anR factor of 0.036. The 4-oxo-1,3-dioxane ring is in a slightly distorted O(1)-sofa conformation flattened at the C(4) end with the 5-isopropyl substituent in a pseudoaxial position and planar lactone group. The molecules form dimers by means of intermolecular N-HO(4) hydrogen bonds of 3.091(2) Å. The1H NMR spectrum of the title compound shows unusual features. 相似文献
97.
Zbigniew J. Jurek 《Journal of multivariate analysis》1983,13(4):578-604
Let
= {Ut: t > 0} be a strongly continuous one-parameter group of operators on a Banach space X and Q be any subset of a set
(X) of all probability measures on X. By
(Q;
) we denote the class of all limit measures of {Utn(μ1 * μ2*…*μn)*δxn}, where {μn}Q, {xn}X and measures Utnμj (j=1, 2,…, n; N=1, 2,…) form an infinitesimal triangular array. We define classes Lm(
) as follows: L0(
)=
(
(X);
), Lm(
)=
(Lm−1(
);
) for m=1, 2,… and L∞(
)=m=0∞Lm(
). These classes are analogous to those defined earlier by Urbanik on the real line. Probability distributions from Lm(
), m=0, 1, 2,…, ∞, are described in terms of their characteristic functionals and their generalized Poisson exponents and Gaussian covariance operators. 相似文献
98.
The determination of tungsten in steels and alloys with the three-electrode direct current plasma (DCP) “spectrajet” was investigated. The relative intensities of 17 spectral lines of tungsten and several possible interfering lines of its concomitants are listed. WI 400.875 nm is normally best suited, because the background produced by iron and acid is low and easily compensated for by using a blank solution. The limit of detection cl in steels is 2 × 10?3% W for 10 of sample. The line W I 407.436 nm is preferred in the presence of much titanium. For the purpose considered the DCP provides about the same power of detection as the more expensive inductively coupled plasma (ICP), but its observation zone is less well buffered against influences from the matrix. 相似文献
99.
We show that if u is a plurisubharmonic function defined on an open subset of 2 then the Monge-Ampère measure (ddcu)2 can be well defined if and only if u belongs to the Sobolev space W1,2loc().Partially supported by KBN Grant #2 P03A 028 19 相似文献
100.
Let K be the field of real or complex numbers. Let (X K2n,) be a symplectic vector space and take 0 < k < n,N =. Let L1,...,LN X be 2k-dimensionallinear subspaces which are in a sufficiently general position.It is shown that if F : X X is a linear automorphism whichpreserves the form k on all subspaces L1,...,LN, then F is ank-symplectomorphism (that is, F* = k, where ). In particular, if K = R and k is odd then F mustbe a symplectomorphism. The unitary version of this theoremis proved as well. It is also observed that the set Al,2r ofall l-dimensional linear subspaces on which the form has rank 2r is linear in the Grassmannian G(l,2n), that is, there isa linear subspace L such that Al,2r = L G(l, 2n). In particular,the set Al,2r can be computed effectively. Finally, the notionof symplectic volume is introduced and it is proved that itis another strong invariant. 相似文献