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991.
In this study, a simple, rapid and sensitive method for the determination of five phthalates including dimethyl phthalate, diethyl phthalate, dipropyl phthalate, benzyl butyl phthalate, and dicyclohexyl phthalate in fruit jellies by LC coupled with MS has been developed. Samples were pretreated by a dispersive SPE method, termed QuEChERS, which is an acronym for quick, easy, cheap, effective, rugged, and safe. The standard calibration curves were linear for all the analytes over the concentration range of 10–250 ng/mL, and the correlation coefficients ranged from 0.9976 to 0.9991. The LODs and LOQs were in the ranges of 0.09–3.68 ng/mL and 0.28–11.25 ng/mL, respectively. The accuracy of this method was evaluated by measuring the recovery from spiked samples. The recoveries of all five phthalates from samples spiked at three different concentrations (0.01, 0.03, and 0.05 mg/kg), were in the ranges of 83.5–103.9%, 86.7–95.8%, and 87.1–95.2%, respectively. The RSD values for the samples spiked at 0.01, 0.03 , and 0.05 mg/kg ranged from 2.0–7.6%, 1.4–6.4%, and 1.2–3.8%, respectively. The method has been used for the analysis of real samples and BBP and DEP were found in real samples. 相似文献
992.
Yuki Shinno Dr. Kenta Iyoki Dr. Koji Ohara Yutaka Yanaba Dr. Yusuke Naraki Prof. Dr. Tatsuya Okubo Prof. Dr. Toru Wakihara 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2020,132(45):20274-20278
The STW-type zeolite is attractive for developing novel enantioselective syntheses/separation of chiral compounds because it is the only chiral zeolitic microporous material whose enantioenriched synthesis has been achieved. In addition to the conventional industries in which zeolites are used, STW should have diverse industrial applications in the pharmaceutical and food industries. However, the toxic and caustic fluoride required for synthesizing STW severely hinders its commercialization by mass production. Herein, we report the first example of fluoride-free STW synthesis, in which the two roles of fluoride—formation of a zeolitic framework rich in tetravalent T-atoms and promotion of double 4-membered ring unit formation—were substituted by dry gel conversion and Ge addition, respectively. The STW obtained was highly crystalline, with a similar micropore volume and thermal stability as those of original fluoride-based STW. Our approach is promising not only for the fluoride-free synthesis of enantiomeric STW but also for general fluoride-free syntheses. 相似文献
993.
A Reagent for the One‐Step Preparation of Potassium Acyltrifluoroborates (KATs) from Aryl‐ and Heteroarylhalides 下载免费PDF全文
Dr. Gábor Erős Yo Kushida Prof. Dr. Jeffrey W. Bode 《Angewandte Chemie (International ed. in English)》2014,53(29):7604-7607
Potassium acyltrifluoroborates (KATs) are fascinating functional groups whose further exploration is limited by poor synthetic access. Documented herein is the design and synthesis of a new reagent for their one‐step preparation from aryl‐ and heteroarylhalides. The reagent is a stable, soluble zwitterion prepared by S‐alkylation of a novel thioformamide trifluoroboronate. The KATs are prepared by adding one equivalent of nBuLi to a mixture of the aryl halide and the reagent at ?78 °C. This protocol is suitable for the preparation of KATs containing pyridines, esters, nitro groups, and halides. 相似文献
994.
We studied the preparation and circular dichroism (CD) behavior of 2,6-pyridylene ethynylene octameric oligomer linked to a β-d-glucoside moiety with a C20-alkylene chain. The addition of Cu(OTf)(2) salt led to a remarkable enhancement of the first CD band of the oligomer, and an unexpected concentration and time dependency were observed. For example, when 1.0 × 10(-3) M of Cu(OTf)(2) was added to a 1,2-dichloroethane solution of the oligomer (5.0 × 10(-4) M, unit concentration), the CD band appeared in the positive at first and gradually inverted into the negative with time. 相似文献
995.
Planarized triarylboranes: stabilization by structural constraint and their plane-to-bowl conversion
Zhou Z Wakamiya A Kushida T Yamaguchi S 《Journal of the American Chemical Society》2012,134(10):4529-4532
Triphenylborane and 9,10-diphenyl-9,10-dihydro-9,10-diboraanthracene, constrained to a planar arrangement with methylene tethers, were synthesized by intramolecular multi-fold Friedel-Crafts cyclization. These compounds were stable toward air, water, and amines, despite the absence of steric protection in the vertical direction with respect to the B atoms, and showed characteristic structural, electronic, and photophysical properties. In addition, upon treatment with a fluoride ion, these compounds underwent a plane-to-bowl conversion in a controlled manner. 相似文献
996.
Nakashima S Ando H Imamura A Yuki N Ishida H Kiso M 《Chemistry (Weinheim an der Bergstrasse, Germany)》2011,17(2):588-597
The hybrid ganglioside X1, which was identified in the bovine brain, was synthesized for the first time. Ganglioside X1 is believed to be involved in the development of amyotrophic lateral sclerosis-like disorders in patients with neurological disorders after treatment with bovine brain gangliosides. A convergent approach using two branched glycan units, the GM2-core trisaccharide and the lacto-ganglio tetrasaccharide, efficiently provided the highly branched heptasaccharide part of ganglioside X1, which was conjugated with the ceramide part to produce the protected ganglioside X1. Global deprotection delivered homogenous ganglioside X1, with which serum from the patient was reacted. 相似文献
997.
In the presence of TMSSnBu(3) and CsF, stannylation of N-Boc- and N-Cbz-α-amido sulfones proceeded very well to afford the corresponding α-amido stannanes in moderate-to-high yields. This reaction tolerated α-aryl-, alkenyl-, and alkyl-substituted α-amido sulfones as well as substrates containing either an ester or cyano moiety, which might be reactive with lithium or magnesium stannides employed in conventional stannylation. 相似文献
998.
Fujikawa K Nakashima S Konishi M Fuse T Komura N Ando T Ando H Yuki N Ishida H Kiso M 《Chemistry (Weinheim an der Bergstrasse, Germany)》2011,17(20):5641-5651
The first synthesis of ganglioside GalNAc-GD1a, featuring efficient glycan assembly and a cyclic glucosyl ceramide as a versatile unit for ganglioside synthesis is described. Although ganglioside GalNAc-GD1a was first found as a brain ganglioside, IgG autoantibodies to GalNAc-GD1a were subsequently found to be closely related to a human peripheral-nerve disorder, Guillain-Barré syndrome, which is the commonest cause of acute flaccid paralysis worldwide. In this study, the characteristic hexasaccharide part carrying two sialic acid residues was synthesized efficiently by use of a readily accessible GM2-core unit as a common unit. The potentially difficult coupling of the oligosaccharide and ceramide moieties was carried out by using a cyclic glucosyl ceramide as a coupling partner for the hexasaccharide part, thereby successfully providing the framework of the target compound. Global deprotection delivered the homogenous ganglioside GalNAc-GD1a. An enzyme-linked immunosorbent assay showed that sera from patients with Guillain-Barré syndrome reacted both with natural and with synthetic GalNAc-GD1a. 相似文献
999.
Efficient electronic structure methods can be built around efficient tensor representations of the wavefunction. Here we first describe a general view of tensor factorization for the compact representation of electronic wavefunctions. Next, we use this language to construct a low-complexity representation of the doubles amplitudes in local second-order M?ller-Plesset perturbation theory. We introduce two approximations--the direct orbital-specific virtual approximation and the full orbital-specific virtual approximation. In these approximations, each occupied orbital is associated with a small set of correlating virtual orbitals. Conceptually, the representation lies between the projected atomic orbital representation in Pulay-Saeb? local correlation theories and pair natural orbital correlation theories. We have tested the orbital-specific virtual approximations on a variety of systems and properties including total energies, reaction energies, and potential energy curves. Compared to the Pulay-Saeb? ansatz, we find that these approximations exhibit favorable accuracy and computational times while yielding smooth potential energy curves. 相似文献
1000.