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1.
An efficient protocol for a one-pot synthesis of mono-sulfonamides has been developed. It features utilization of excess of sulfonylating agent followed by base mediated recovery of the primary sulfonamide. 相似文献
2.
Dimethyl carbonate synthesis via transesterification catalyzed by quaternary ammonium salt functionalized chitosan 总被引:2,自引:0,他引:2
Yuan Zhao~ 《中国化学快报》2008,19(3):286-290
A quaternary ammonium salt covalently linked to chitosan was first used as a catalyst for dimethyl carbonate (DMC) synthesis by the transesterification of propylene carbonate (PC) with methanol. The effects of various reaction variables like reaction time, temperature and pressure on the catalytic performance were also investigated. 54% DMC yield and 71% PC conversion were obtained under the optimal reaction conditions. Notably, the catalyst was able to be reused with retention of high catalytic activity and selectivity. Consequently, the process presented here has great potential for industrial application due to its advantages such as stability, easy preparation from renewable biopolymer, and simple separation from products. 相似文献
3.
[reaction: see text] Asymmetric diol boronic esters with potassium bifluoride form the corresponding alkyltrifluoroborate and free diol under mild conditions. Defluoridation with tetrachlorosilane produces an alkyldifluoroborane intermediate. This conversion of relatively unreactive boronic esters to derivatives that are strong Lewis acids opens new synthetic opportunities, as illustrated by the preparation of (R)-2-phenylpyrrolidine in 98% ee from a pinanediol or 1,2-dicyclohexyl-1,2-ethanediol boronic ester via potassium (2-phenyl-4-azidobutyl)trifluoroborate. 相似文献
4.
This paper describes a simple chiral primary amine-catalyzed highly efficient and practical protocol for the synthesis of both Wieland-Miescher ketone and Hajos-Parrish ketone as well as their analogues. The reaction can be conducted in gram scale with 1% mol catalyst loading producing high enantioselectivity (up to 96% ee) and excellent yields (up to 98%). This procedure represents one of the most efficient methods for the synthesis of these versatile chiral building blocks. 相似文献
5.
Lanthanide orthochromites of general formula LnCrO3 (Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Tb, Lu) and YCrO3 have been made by self-propagating high-temperature synthesis (SHS). Four different SHS reactions were found to form LnCrO3: reaction of Ln2O3, Cr and CrO3 with NaClO4 or Ba (ClO4)2 in air; reaction of Ln2O3, Cr and CrO3 in oxygen; reaction of LnCl3, CrCl3 and NaO2 or Na2O2 in air and reaction of Ln (NO3)3, Cr and melamine in air. Reactions were studied by DTA and TGA experiments which showed exotherms and weight losses associated with the initiation temperatures (ca. 350°C) of the SHS reactions. Maximum reaction temperature Tc and propagation velocity Uc were measured for selected reactions. X-ray powder diffraction showed a single phase orthorhombic perovskite structure was produced in all reactions. Systematic changes in the lattice parameters, cell volume and pycnometrical densities were seen as a function of lanthanide atomic number. SHS prepared LnCrO3 samples were all shown to be weak antiferromagnets. IR spectra for the LnCrO3 materials showed bands at 635, 480, 440, 350 and 180 cm−1. 相似文献
6.
Buchstaller HP 《Journal of combinatorial chemistry》2003,5(6):789-793
The first solid-phase synthesis of oxazolidinones by cycloaddition of resin-bound epoxides with isocyanates is described. Synthesis of the title compounds was achieved by alkylation of resin-bound carbamates with glycidyl tosylate, followed by cycloaddition of the resulting epoxides with isocyanates at elevated temperature in high yields and purity. Because N-aryloxazolidinones have been known to possess various biological activities, this method is useful from the viewpoint of drug discovery. 相似文献
7.
8.
B. I. Martynov V. B. Sokolov A. Yu. Aksinenko T. V. Goreva T. A. Epishina A. N. Pushin 《Russian Chemical Bulletin》1998,47(10):1983-1984
A convenient method was developed for the synthesis of the lithium salt of 1,1-bis(diethoxyphosphoryl)fluoromethane from availableO,O-diethyl (chlorofluoromethyl)phosphonate, and some transformations of the resulting salt were studied.
Dedicated to the memory of Academician M. I. Kabachnik on his 90th birthday.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 2039–2040, October, 1998. 相似文献
9.
The closure by cyclization with diethyl carbonate (EtO)(2)CO from aminoalcohols 1 as starting material can lead to the oxazolidinones 2a, b and 2c, respectively. In the reaction of trans-isomer (6) and (EtO)(2)CO, isolated products were also only 5-membered oxazolidinone derivative (7), containing its dehydrated derivative 8. The preferential formation of the 5-membered oxazolidinone ring system apparently indicated that this process (5-Exo-Trig ring closure) is more favorable than that of 6- or 7-membered ring derivative (3 or 9) by 6- or 7-Exo-Trig ring closure. 相似文献
10.
Porphine formation from pyrrole and formaldehyde was examined in detail. Under optimized conditions, 9 mg of crystalline porphine was obtained per 1 ml of pyrrole. 相似文献
11.
12.
There are many examples of both naturally occurring and synthetic molecules containing a 2-oxazolidinone ring that have significant biological activity. The oxazolidinone ring potentially has three sites for attachment of diversity elements. A synthesis that can provide for inclusion of diversity elements at all three positions should be a powerful method for the preparation of oxazolidinone libraries. In this paper we present the preparation of a 3 x 3 x 3 array yielding 27 different products with minimal workup, high yields, and, most importantly, high purity. Using an intramolecular acylnitrene-mediated aziridination reaction, we have prepared (triphenylmethoxymethyl)-3-oxa-1-azabicyclo[3.1.0]hexan-2-one as a starting material for library generation. The first substitution involves opening the aziridine ring of the azabicyclo[3.1.0]hexane ring system using a Grignard reagent. The nitrogen of the oxazolidinone is now ready for substitution via alkylation or arylation. Removing the trityl protecting group via esterification under mildly acidic conditions accomplishes the final substitution. 相似文献
13.
Alexander Steblyanko Wonmun Choi Fumio Sanda Takeshi Endo 《Journal of polymer science. Part A, Polymer chemistry》2000,38(13):2375-2380
A bifunctional five‐membered cyclic carbonate was synthesized from carbon dioxide and diglycidyl terephthalate, and its polyaddition with alkyl diamines were carried out in DMF at room temperature to obtain the corresponding poly(hydroxyurethane)s with Mn s in the range of 6300–13200 in good yields. The structures of the obtained polymers were confirmed by IR and NMR spectroscopy and their glass‐transition and decomposition temperatures were observed at 3–29 °C and 182–277 °C, respectively. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 2375–2380, 2000 相似文献
14.
Yu. V. Ostapiuk V. S. Matiichuk N. I. Pidlypnyi N. D. Obushak 《Russian Journal of Organic Chemistry》2012,48(4):519-522
A simple and convenient procedure was proposed for the synthesis of 4-aryl-3-bromobutan-2-ones from methyl vinyl ketone and
arenediazonium bromides under Meerwein reaction conditions. 相似文献
15.
J Wang A Sugawara-Narutaki A Shimojima T Okubo 《Journal of colloid and interface science》2012,379(1):41-47
Evanescent wave-cavity ring-down spectroscopy (EW-CRDS) is employed to characterize micellization of anionic surfactants and the related capability of removing cationic substance off the silica surface. Crystal violet (CV(+)) cationic dye is used as a molecular probe to effectively determine critical hemimicelle concentration (HMC) of surfactants on the surface. The HMC results are 1×10(-2), 4×10(-3), 8×10(-4), and 2.5×10(-4) mol/L for sodium sulfate salts with a carbon-chain length of C-10, C-12, C-14, and C-16, respectively. A stronger hydrophobic interaction results in a less concentration required to undergo micellization. The HMC values on the surface are about half of those in solution. When NaCl solution is added, the electrolyte helps reduce the electrostatic repulsion between the anionic sulfate heads to facilitate the surfactant aggregation, and thus, the subsequent HMC is reduced. Furthermore, the probable phase change for dye-surfactant interactions on the surface at the concentration below HMC is observed, and the desorption rates of CV(+) are measured as a function of concentration and carbon-chain length of surfactants above HMC. Given each surfactant concentration at its respective HMC, the corresponding desorption rates are along the order of C-12相似文献
16.
《Tetrahedron letters》1987,28(25):2857-2860
17.
Adrian S. Culf Jennifer A. Melanson Rodney J. Ouellette Glen G. Briand 《Tetrahedron letters》2012,53(26):3301-3304
This Letter details the particular use of salicylaldehyde (2-hydroxybenzaldehyde) for the regiospecific protection of primary amines in a representative polyamine, norspermidine (N-(3-aminopropyl)propane-1,3-diamine) under mild reaction conditions in high yield. The lack of intramolecular hexahydropyrimidine formation allowed for subsequent N2-acylation and N2-alkylation reactions, typical of polyamine synthetic strategies. 相似文献
18.
丙氨酰-谷氨酰胺的简便有效合成 总被引:2,自引:0,他引:2
谷氨酰胺 (Gln)是肠道必需氨基酸 ,是肠粘膜细胞氧化的重要燃料。肠粘膜缺乏Gln将严重损伤肠屏障功能 ,创伤性休克及化疗应激可加重损害 ,导致肠粘膜萎缩 ,肠道细菌移位 ,甚至促发脓毒症和多器官功能不全 (MODS) [1] 。但Gln性质不稳定 ,不能耐高温消毒 ,因此 ,一般氨基酸制剂不含Gln。Ala Gln为Gln代谢前体 ,溶解度高 ,性质较Gln稳定 ,能耐受热灭菌 ,在体内数分钟即分解出Gln ,能部分补偿肠道所需Gln ,减少严重创伤及腹腔注射化疗药物 5 氟尿嘧啶 (5 FU)引发的小肠粘膜形态功能改变 ,细菌移位 ,降低… 相似文献
19.
Naoto Aoyagi Yoshio Furusho Takeshi Endo 《Journal of polymer science. Part A, Polymer chemistry》2013,51(5):1230-1242
Hydroiodides of secondary and primary amines effectively catalyzed the reaction of carbon dioxide and epoxides under mild conditions such as ordinary pressure and ambient temperature, to obtain the corresponding five‐membered cyclic carbonates in moderate to high yields. Detailed investigation showed that the catalytic activity was highly affected by the counter anions of the ammonium salts; the iodides catalyzed efficiently the carbonate‐forming reactions, whereas the bromide and chloride counterparts exhibited almost no catalysis. We also revealed that two important factors on the amine moieties that affected the catalytic reactions. First, the catalytic activity increased with increasing bulkiness of the substituents on the ammonium nitrogen atoms. Second, the catalysis became more efficient as the parent amines become more basic. Dicyclohexylammonium iodide was the best catalyst among the ammonium salts investigated in this study. As an application of this reaction system, we synthesized homo‐ and copolymers bearing epoxide pendant groups as substrates, which were converted with high efficiency into the corresponding homo‐ and copolymers bearing cyclic carbonate pendant groups under 1 atm at 45 °C. All polymers were easily purified simply by precipitation in water, and were isolated in high yields (>95%). © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2013 相似文献
20.
A one-pot, three-component condensation of a carbonyl compound, an amine and a nitroalkene leading to an efficient synthesis of alkyl-substituted pyrroles has been carried out in molten tetrabutylammonium bromide. Neither a catalyst nor an organic solvent is required for this reaction and the molten ammonium salt is recyclable. 相似文献