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91.
It was previously reported that methyl oleanonate (5) and lanost-8-en-3-one (10) give predominantly [3,2-c]isoxazoles. On the contrary, we have confirmed that both compounds 5 and 10 do not give [3,2-c]isoxazoles but rather afford regioselectively [2,3-d]isoxazoles in good yields. Consequently, a new lanostane triterpenoid with a cyano-enone functionality in ring A was synthesized in two steps from the corresponding [2,3-d]isoxazole, which is interesting from the perspective of biological activity because lanosterol is the biogenetic precursor of steroids. 相似文献
92.
Yoshimatsu K Kiuchi F Shimomura K Makino Y 《Chemical & pharmaceutical bulletin》2005,53(11):1446-1450
A rapid and reliable solid-phase extraction method for HPLC analysis of opium alkaloids from Papaver plants was established. Fifty mg of dried and powdered plant sample was extracted with 5 ml of 5% acetic acid for 30 min under sonication. After centrifugation, 3 ml of the supernatant was loaded on a reversed-phase cation-exchange solid-phase extraction cartridge. After seriate washings with 0.1 M hydrochloric acid and methanol, alkaloids were eluted with a mixture of 28% ammonia and methanol (1:19). The eluate was concentrated under nitrogen stream at 40 degrees C and the residue was dissolved in 50% aqueous methanol for high performance liquid chromatographic analysis. With this solid-phase extraction method, the recovery of morphine, codeine, oripavine, thebaine, papaverine, noscapine and sanguinarine was from 99.94 to 112.18% when the standard alkaloids were added to the plant samples. Opium alkaloids of a variety of genus Papaver plants cultivated in a field and phytotron were analyzed by this method. 相似文献
93.
Separation of the enantiomers and diastereomers of ephedrines was investigated for impurity profiling of methamphetamine. We describe a method for the analysis of (1S,2R)-(+)-ephedrine, (1R,2S)-(-)-ephedrine, (1S,2S)-(+)-pseudoephedrine and racemic methylephedrine in bulk methamphetamine by HPLC using two different columns: a phenyl-beta-cyclodextrin-type column and an ODS-type column. The analytes were detected by UV absorbance measurement at 210 nm. As little as 0.05% of each ephedrine in bulk methamphetamine could be determined. In the impurity profiling of methamphetamine, the identification of ephedrines may provide valuable information about the precursor. This method was confirmed to be sufficiently sensitive to identify trace amounts of (1R,2S)-(-)-ephedrine and (1S,2S)-(+)-pseudoephedrine in bulk methamphetamine synthesized by the Emde method. 相似文献
94.
Jun Takahashi Kazuto Kawakami Yukiko Kobayashi 《Surface and interface analysis : SIA》2019,51(1):12-16
Although steel research has a very long history, there are still various questions and uncertainties on the fundamental issues of steel materials. Our aim is to clarify the issues by atomic-scale characterization using atom probe tomography (APT). This paper introduced our developed techniques in application of APT into steel materials. The first one is the specimen tip preparation technique from the site-specific regions of interest in steel, which significantly expanded the application field of steel analysis. The second one is the observation technique of trapped hydrogen in steel using our developed “deuterium charge cell,” which accomplished direct observation of the hydrogen trapping site in alloy carbide precipitation strengthened steels. Such atomic-scale analyses bring many new findings in steel materials science. 相似文献
95.
Dr. Kento Ishida Hokuto Yamazaki Chihiro Hagiwara Prof. Dr. Manabu Abe Prof. Dr. Hiroyuki Kusama 《Chemistry (Weinheim an der Bergstrasse, Germany)》2020,26(6):1249-1253
Acylsilanes have been known to undergo isomerization to siloxycarbenes under photoirradiation and the thus generated carbenes can be utilized for various synthetic reactions. But this carbene formation is not necessarily efficient with some alkanoylsilanes because Norrish-type fragmentations compete, which limit the synthetic utility of alkanoylsilanes as carbene precursors. In this study, generation of siloxycarbenes from alkanoylsilanes by visible-light-induced energy transfer was examined by using an Ir complex, [Ir{dF(CF3)ppy}2(dtbpy)]PF6, and was successfully applied to the C−C coupling reactions with boronic esters or aldehydes. This methodology efficiently suppressed undesired Norrish-type reactions and broadened synthetic utility of alkanoylsilanes. 相似文献
96.
Takahashi Hiroaki Park Ki Chul Nomura Masao Shibahara Hiroki Miura Hanako Ohishi Yukiko Yuki Mami Tsukahara Takehiko 《Journal of Radioanalytical and Nuclear Chemistry》2021,329(1):327-336
Journal of Radioanalytical and Nuclear Chemistry - The influence of extraction process on Cs isotope ratios was investigated by thermal ionization mass spectrometry (TIMS) for nitric-acid (HNO3)... 相似文献
97.
Yukiko Enomoto Hiroshi Kamitakahara Toshiyuki Takano Fumiaki Nakatsubo 《Cellulose (London, England)》2006,13(4):437-448
Novel cellobiose and cellulose (DP
n
=ca. 30) derivatives, N-(1-pyrenebutyloyl)-4-O-(β-d-glucopyranosyl)-β-d-glucopyranosylamine (6), N-(15-(1-pyrenebutyloylamino)-pentadecanoyl)-4-O-(β-d-glucopyranosyl)-β-d-glucopyranosylamine (7), N-(1-pyrenebutyloyl)-β-cellulosylamine (13), N-(15-(1-pyrenebutyloylamino)-pentadecanoyl)-β-cellulosylamine (14) carrying a pyrene group as a single fluorescent probe at the reducing end, were prepared in order to investigate their self-assembly systems in solutions. The relative intensity of the excimer emission at ca. 480 nm due to dimerized pyrenes (intensity I
E) to the monomer emission at ca. 380 nm due to isolated pyrene (intensity I
M), i.e., I
E/I
M, was monitored in various solutions. In water/dimethyl sulfoxide (DMSO) mixed solvent (0–98%, v/v), the ratio I
E/I
M remained low (0.04) for compound 6 over the range of water concentrations, indicating that pyrenes at C-1 position of compound 6 were diffused. On the other hand, the ratio I
E/I
M increased (0.04–4.96) for compound 7 with the increase in water concentration, indicating that pyrenes at C-1 position were associated. In aqueous NaOH solutions (4.4–17.5%, w/w), compound 14 showed a large increase in the ratio I
E/I
M (0.84–8.14) with the increase in NaOH concentration, compared to compound 13 (0.06–0.41). It was found that the association of hydrophobic groups at the reducing-end of cellulose could be controlled by the hydrophilic–hydrophobic balance of compounds and the solvent polarity. 相似文献
98.
Liquid‐Crystalline Biomacromolecular Templates for the Formation of Oriented Thin‐Film Hybrids Composed of Ordered Chitin and Alkaline‐Earth Carbonate
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Dr. Tatsuya Nishimura Ken Toyoda Takahiro Ito Dr. Yuya Oaki Yukiko Namatame Prof. Takashi Kato 《化学:亚洲杂志》2015,10(11):2356-2360
Macroscopically ordered inorganic thin films have been formed on unidirectionally oriented, liquid‐crystalline chitin matrices. In the presence of poly(acrylic acid) (PAA), unidirectionally oriented chitin films act as templates for the formation of oriented thin‐film crystals of alkaline‐earth carbonates such as SrCO3 and BaCO3. The morphology and orientation of crystals are dependent on the metal ion concentration. For SrCO3 crystallization, unidirectional thin films and hexagonal‐shaped thin films have been deposited from 200 and 25 mm concentration strontium solutions, respectively. 相似文献
99.
100.