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991.
Novel unsymmetrical vanadyl and zinc dodecakis(2,2,2‐trifluoroethoxy)phthalocyaninates with an iodo group were synthesized by a statistical condensation route. The palladium‐catalyzed coupling reaction between such monoiodinated metallophthalocyanines and terminal acetylenic derivatives gave various new unsymmetrically dodecakis(2,2,2‐trifluoroethoxy)‐substituted metallophthalocyanines with extended exocyclic π‐conjugation. Unsymmetrical zinc dodecakis(2,2,2‐trifluoroethoxy)phthalocyaninate with a nitro group was also prepared for comparison. All the target phthalocyanines were separated by common col umn chromatography and characterized by elemental analysis, ir and 1H‐nmr, uv‐visible and fast‐atombombardment mass spectroscopy. 相似文献
992.
Jun-ichi Matsuo Ryosuke Okuno Kosuke Takeuchi Mizuki Kawano Hiroyuki Ishibashi 《Tetrahedron letters》2010,51(29):3736-3737
Optimized reaction conditions for the preparation of various 2-monosubstituted 3-ethoxycyclobutanones are described. 2-Monoalkyl 3-ethoxycyclobutanones were efficiently prepared by the reaction of the corresponding carboxylic acid chlorides and an excess amount of ethyl vinyl ether in the presence of diisopropylethylamine at 90 °C in a sealed tube. 2-Monoaryl 3-ethoxycyclobutanones were prepared by using 2,6-lutidine as a base in the above-mentioned procedure. 相似文献
993.
994.
Yusuke Iwasaki Masato Goto Keisuke Mochizuki Emi Terayama Rie Ito Koichi Saito Norihiro Sugino Tsunehisa Makino Hiroyuki Nakazawa 《Biomedical chromatography : BMC》2011,25(4):503-510
A selective and sensitive HILIC‐MS/MS method for the simultaneous quantification of nicotine and its metabolites in human maternal and cord sera was developed and validated. After solid‐phase extraction, LC separation was achieved on a hydrophilic interaction chromatography. The validated method is capable of selective identification as well as accurate and sensitive quantification. Analyte recovery ranged from 86.2 to 107.7% and intra‐ and inter‐day assay precision were less than 15% relative standard deviation. This sensitive HILIC‐MS/MS method can be used to determine nicotine and its metabolic profile in smokers. This validated method is useful for the determination of nicotine and its metabolites in human serum in future studies of the effects of nicotine exposure on neonatal outcome. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
995.
996.
Norihisa Fukaya Hisato Haga Syun-ya Onozawa Hiroyuki Yasuda 《Journal of organometallic chemistry》2010,695(23):2540-2542
Organic functionalization of a silica surface has been realized by employing arylsilanes. Grafting reactions of aryl(3-chloropropyl)dimethylsilanes (aryl = p-anisyl, p-tolyl, phenyl) with silica were carried out in heptane at 80 °C for 24 h. The 29Si and 13C CP/MAS spectra of the obtained silica materials clearly showed that the 3-chloropropyldimethylsilyl moieties were cleanly grafted onto silica via a siloxane (Si-O-Si) bond accompanied by the release of the aryl groups. The loading amounts on FSM-type mesoporous silica (TMPS-4) with aryl(3-chloropropyl)dimethylsilanes were comparable to those with 2-propenylsilane and the most commonly used methoxysilane. 相似文献
997.
F. Sato Y. Tanimura T. Tanaka T. Iida T. Yamauchi K. Oda 《Radiation measurements》1999,31(1-6):253-256
A CR-39 track detector was successfully used to measure the outline of thin low-energy ion beams. After the etching, the surface of the detector was examined with an observation system composed of a Normarski microscope, a CCD camera and a digital image processing computer. Beam images obtained with the system were in good agreement on the outline of the beam formed with a beam aperture. Also, the resolving power in the beam outline measurement was roughly explained from the consideration of the ion range and the etch-pit growth in the chemical etching for the CR-39 detector. 相似文献
998.
999.
The nucleophilic substitution reaction by gas-solid contact has been investigated. When 9-thienothienylfluoren-9-ol derivatives were coground with dichlorodicyanoquinone (DDQ) and then exposed to methanol vapor, the corresponding 9-methoxyfluorenes were obtained in 15-70% yields. Throughout the whole procedure the solid state was retained. The generation of a radical cation in the coground solids via charge-transfer interaction between the substrate alcohol and DDQ was suggested by the ESR spectrum. The mechanism involving the collapse of the radical cation to generate a proton, which acts as a catalyst to afford the carbocation, was deduced based on the electrochemical oxidation of the substrate in solution. The propagation of the substitution reaction in the solid state has been shown for the carbocation upon contact with methanol vapor. The crystalline inclusion compounds of 9-thienothienylfluoren-9-ol derivatives incorporating methanol as a guest were exposed to HCl gas. This gas-solid reaction also led to the formation of the corresponding methoxy compounds maintaining the solid state. Through this work a new consequence of solid-state cogrinding is deduced. 相似文献
1000.