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1.
Andrzej Piasecki 《Monatshefte für Chemie / Chemical Monthly》1986,117(11):1287-1293
2-(2-Alkoxyethyl)-1,3-dioxanes (1) were prepared by ap-toluenesulfonic acid-catalyzed, one-step reaction of propenal with a mixture of aliphatic alcohol and trimethylene glycol in good yields. The transacetalization reaction of 1,1,3-trialkoxypropanes (3) with ethylene glycol or propylene-(1,2)glycol afforded good yields of pure 2-(2-alkoxyethyl)-1,3-dioxolanes (5 or6), respectively. This reaction proceeds through an intermediate 1,3-dialkoxy-1-(2-hydroxyalkoxy)-propane.
Ein- oder Zweistufensynthese von 2-(2-Alkoxyethyl)-1,3-dioxacyclanen
Zusammenfassung In der durchp-Toluolsulfonsäure — katalysierten, direkten Reaktion von Propenal mit einem Gemisch von aliphatischem Alkohol und Trimethylenglykol wurden die entsprechenden 2-(2-Alkoxyethyl)-1,3-dioxane (1) in guten Ausbeuten erhalten. Die Umacetalisierung von 1,1,3-Trialkoxypropanen (3) mit Ethylenglykol oder 1,2-Propylenglykol lieferte 2-(2-Alkoxyethyl)-1,3-dioxolane (5 oder6) in guten Ausbeuten. Die Umacetalisierungsreaktion von 1,1,3-Trialkoxypropanen verläuft über 1,3-Dialkoxy-1-(2-hydroxyalkoxy)-propane als Zwischenprodukte.相似文献
2.
M. Judith Percino Víctor M. Chapela Omar Urzúa Ling-Fa Montiel Cecilia Rodríguez-Barbarín 《Research on Chemical Intermediates》2007,33(7):623-629
The novel intermediate 1-(p-fluorophenyl)-2-(2′-pyridyl)ethanol or 2-[2′-(1-hydroxy-1-(p-fluorophenyl)ethyl]pyridine and the corresponding novel dehydration compound 1-(p-fluorophenyl)-2-(2′-pyridyl)ethene or 2-[p-fluorophenylvinyl]pyridine were obtained from the condensation reaction of p-fluorophenylaldehyde and 2-picoline under catalyst-and solvent-free conditions. The intermediate 1-(p-fluorophenyl)-2-(2′-pyridyl)ethanol was obtained at 42 h reaction time and temperature of 120°C, respectively. 1H-NMR, IR spectroscopic data of the 1-(p-fluorophenyl)-2-(2-pyridyl)ethanol clearly showed the presence of the-CH2-CHOH-group. The compound was obtained as a white powder with m.p. 121–122°C and a yield of 8%. For 1-(p-fluorophenyl)-2-(2-pyridyl)ethene, the reaction conditions were similar, but the reaction temperature was increased to yield
the double bond in the 1-(p-fluorophenyl)-2-(2′-pyridyl)ethene. At the reaction temperature of 140°C, the compound was a slightly brown powder with a
m.p. of 78°C and yield of 18%. 1H-NMR, IR spectroscopic data for the 1-(p-fluorophenyl)-2-(2′-pyridyl)ethene showed the presence of a double bond in trans configuration (-CH=CH-), characteristic of a styrylpyridine. 相似文献
3.
Stereoselective diazotization of (S)-2-amino-2-phenyl acetic acid (L-phenyl glycine) (4) with NaNO2 in 6% H2SO4 in a mixture of acetone and water gave optically pure (S)-2-hydroxy-2-phenyl acetic acid (L-mandelic acid) (5). Esterification, gave (S)-2-hydroxy-2-phenyl acetic acid esters (6). The latter was treated with chloroacetyl chloride in the presence of triethylamine (TEA) in dichloromethane (DCM) to yield (S)-2-chloroacetyloxy phenyl acetic acid ester (2). In another sequence, the reaction of 2-(chloromethyl)-3-arylquinazolin-4(3H)-one (9) treated with N-Boc piperazine, followed by deprotection of the Boc group, to obtain 3-aryl-2-((piperazin-1-yl)methyl) quinazolin-4(3H)-one (3). Reaction of 2 with 3 in the presence of K2CO3 and KI gave the title compound, 2-(2-(4-((3,4-dihydro-4-oxo-3-arylquinazolin-2-yl)methyl)piperazin-1-yl) acetoyloxy)-2-phenyl acetic acid esters (1). The structures of all the new compounds obtained in the present work are supported by spectral and analytical data. 相似文献
4.
新型2-(2'-取代亚肼基)-1,3-二硫杂环戊烷衍生物的合成和菌活性研究 总被引:3,自引:0,他引:3
通过结构改造并结合活性基团的拼接合成了11个未见文献报道的新型2-(2'-取代亚肼基)-1,3-二硫杂环戊烷类化合物, 所有的目标物的结构都经1H NMR, MS, IR和元素分析证实, 选择了其中5个化合物对7种细菌进行了抑菌活性测试, 并与市售农药20%三环唑、70%威尔达甲托的抑菌活性进行对比, 发现它们比市售农药有更为广泛的杀菌谱, 对照农药只对金黄色葡萄球菌有良好的抑菌作用而这些化合物则对所选择的七个菌种均有良好的抑菌作用. 其中化合物2-(对氟苯氧乙酰亚肼基)-1,3-二硫杂环戊烷(4c)的杀菌谱很广, 它对金色葡萄球菌、大肠杆菌、白色念珠菌的抑杀活性都很好. 相似文献
5.
Yanjun Chen Weiwei Zuo Shu Zhang Wen-Hua Sun 《Journal of organometallic chemistry》2008,693(4):750-762
A series of chromium(III) complexes bearing 2-(1-isopropyl-2-benzimidazolyl)-6-(1-(arylimino)ethyl)pyridines were synthesized and characterized by IR spectroscopic and elemental analysis. The X-ray crystallographic analysis revealed a distorted octahedral geometry of the chromium complexes. When activated by Et2AlCl, MAO or MMAO, these chromium complexes exhibited catalytic activities for ethylene oligomerization and polymerization; while the good to high activities (up to 3.95 × 106 g mol−1 (Cr) h−1) were observed in the catalytic systems with MMAO. Therefore, various reaction parameters of the catalytic system with MMAO were investigated in detail. The steric and electronic effects of ligands affected the catalytic activities and the distribution of the products predominantly. Interestingly, sometimes their distributions of oligomers did not resemble the rules of Schulz-Flory or Poisson due to the hexenes produced in low yield. 相似文献
6.
M.Yu. Dmitrichenko A.V. IvanovI.A. Bidusenko I.A. UshakovA.I. Mikhaleva B.A. Trofimov 《Tetrahedron letters》2011,52(12):1317-1319
1-Vinylpyrrole-2-carbaldehydes react with phosphorus pentachloride (benzene, 10-15 °C) to afford E-2-(2-dichloromethylpyrrol-1-yl)vinylphosphonium hexachlorophosphates in up to 85% yield, which after treatment with SO2 (benzene, rt) are converted into E-2-(2-dichloromethylpyrrol-1-yl)vinylphosphonyl dichlorides in 50-75% yields. 相似文献
7.
8.
有机相酶催化拆分制备(S)-2-氯-1-(2-噻吩)-乙醇 总被引:1,自引:0,他引:1
首次在有机相中对酶催化条件下的2-氯-1-(2-噻吩)-乙醇的反应进行了研究. 通过对不同来源酶的筛选, 找到了Novozym 435和Alcaligenes sp两种选择性较好的酶, 它们均对该反应具有较高的选择性和较快的反应速度, 在此基础上进一步通过对溶剂、温度、摇床转速以及酶用量的筛选, 确定了能够有效拆分2-氯-1-(2-噻吩)-乙醇的较佳反应条件. 当温度35 ℃, 酶量10 mg/mL, 反应72.5 h, 产物的ee值为98.5%时收率为48.6%. 相似文献
9.
Nina A. Nedolya Ol’ga A. Tarasova Alexander I. Albanov Boris A. Trofimov 《Tetrahedron letters》2010,51(40):5316-3368
Substituted N-[2-(vinyloxy)ethyl]pyrroles, prepared in good yield through an allenic or acetylenic carbanion/isothiocyanate one-pot methodology from 2-(vinyloxy)ethyl isothiocyanate and allyloxyallene, methoxyallene, N,N-dimethyl-2-propyn-1-amine, and 3-methoxy-1-(methylsulfanyl)-1-propyne, are smoothly converted into the corresponding N-vinylpyrroles using t-BuOK/DMSO (room temperature). The reaction proceeds via elimination of vinyl alcohol from the N-[2-(vinyloxy)ethyl] substituent and represents a novel approach to N-vinylpyrroles. 相似文献
10.
合成了三[2-(2'-肟亚甲基苯氧基)乙基]胺, 测定了其IR, NMR和单晶结构, 晶体C27H30N4O6属三斜晶系, 空间群R-3r, 晶胞参数为: a=1.9100(2) nm, b=1.9100(2) nm, c=1.9100(2) nm, =109.500(2), =109.500(2). =109.500(2), Z=6. 结构解析最终一致性因子R1=0.0568, wR2=0.1766. 分子间通过氢键和范德华力形成3D网状超分子结构. 使用HyperChem6.0程序中半经验ZINDO/1方法和G98量子化学程序包, 在B3LYP/6-311G**基组水平上对化合物电荷分布进行了量子化学计算. 相似文献
11.
A new thiazolylazo chromogenic reagent, 2-[2-(6-methylbenzo-thiazoly)azo]-5-diethylaminobenzoic acid (6-Me-BTAEB), has been synthesized. Its chromogenic reaction with microamounts of nickel in the presence of sodium dodecylsulfate (SDS) has been thoroughly studied. 6-Me-BTAEB reacts with nickel(II) in weak acid medium containing appropriate amounts of SDS to form a blue-violet complex with high sensitivity, good selectivity and high stability. The composition is found to be 1:2 (nickel to 6-Me-BTAEB) and its absorption maximum is at 650 nm with an apparent molar absorptivity of 1.67 × 105l mole–1 cm–1. Beer's law is obeyed over the range 0-0.4 g of nickel per ml. The proposed method has been applied to the direct determination of nickel in aluminium alloys, pure magnesium and low alloy steels at the 0.2–0.3% (w:w) level with satisfactory results. 相似文献
12.
N. Tonkikh A. Strakovs M. Petrova V. V. Chernyshev H. Schenk 《Chemistry of Heterocyclic Compounds》2002,38(6):724-729
The reaction of 2-aminocarbonyl-5,5-dimethyl-1,3-cyclohexanedione with 2,3-diaminopyridine, 1,2-phenylenediamine (and its 4-methyl, 4-nitro, 4-carboxy, and 4-benzoyl derivatives), and 3,3-diaminobenzidine gave the corresponding 2-[2-(2,3-dihydrobenzimidazolylidene)]- and 2-[2-(2,3-dihydropyrido[2,3-d]imidazolylidene)]-5,5-dimethyl-1,3-cyclohexanediones. Their structure was confirmed by 1H NMR spectroscopic data and X-ray analysis. 相似文献
13.
《Analytical letters》2012,45(7-8):713-723
Abstract Hafnium(IV) reacts with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol in the pH range 3.3–11.0 to yield a sparingly soluble red-coloured chelate that can be dissolved with Triton X-100. Effect of initial pH of metal ion and order of addition of reagents was studied in detail. The 1:3 complex adheres to Beer's law over the concentration range 0.02–1.12 μg/ml of Hf(IV), has a molar absorptivity 1.33x105 1 mol?1cm?1, Sandell sensitivity 1.3 ng cm?2, formation constant (log K) 11.94 and the method had a relative standard deviation of ± 1.5%. Effect of 60 diverse ions on the determination of hafnium(IV) was studied. This fairly selective method is the most sensitive so far reported for the spectrophotometric determination of hafnium(IV). 相似文献
14.
S. Tasqeeruddin P. K. Dubey 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):128-134
Abstract 3-(2-Bromoacetyl)coumarins (I), when treated with 2-mercatobenzimidazole (II) in acetone containing K2CO3 (mild base) and tetrabutylammonium bromide (TBAB) as a phase transfer catalyst, at room temperature yielded the title compound 3-[2-(1H-benzimidazole-2-yl-sufanyl)-acetyl]-chromen-2-one (III) in a one-pot synthesis. Alternatively, III could also be prepared by treating dithiocarbonic acid O-ethyl ester, S-[2-oxo-2-(2-oxo-2H-chromen3-yl)-ethyl] ester (V), with o-phenylenediamine (VI). The methylation of the title compound III was performed with dimethyl sulfate (DMS), in acetonitrile containing TBAB and K2CO3 at room temperature, resulting in 3-[2-(N-methyl-benzimidazol-2-yl-sulfanyl)]-acetyl-chromen-2-ones (VII). Alternatively, methylation of III could also be performed with DMS in acetonitrile containing K2CO3 as base and clay as surface catalyst. All the compounds were synthesized in good yields and their structures were confirmed by spectral and analytical data. [Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental resource: 1H NMR of IIIB, VB and VIIB] 相似文献
15.
Cis-l-acetyl-2-aryl-6,6-dimethyl-5,7-dioxo-spiro-[2,5]-4,8-octadiones 3a-d (X=p-CH3, p-Cl, H, p-NO2) reacted with anhydrous methanol in a sealed tube at 80°C to form trans, cis-α-carbomethoxy-β-(α′-methoxy-α′-aryl)-γ-methoxy-γ-methyl-γ-butyrolactones 4a-d and cis, cis-α-carbomethoxy-β-(α′-methoxy-α′-aryl)-γ-methoxy-γ-methyl-γ-butyrolactones 5a-d in good yield. 相似文献
16.
A variety of functionalized 6-(trifluoromethyl)-6H-dibenzo[b,d]pyrans were easily synthesized in good yields under mild conditions by a domino reaction of 3-nitro-2-(trifluoromethyl)-2H-chromenes with 2-(1-phenylethylidene)- and 2-(1-phenylpropylidene)malononitriles. In the latter case, intermediate 7-amino-10-methyl-10-nitro-9-phenyl-6-(trifluoromethyl)-10,10a-dihydro-6H-benzo[c]chromene-8-carbonitriles were isolated as a result of a rare [1,5] sigmatropic shift of the nitro group. 相似文献
17.
An alternate approach to 2-(substituted phenyl)-3,3a-dihydro-8H-pyrazolo[5,l-a] isoindol-8-ones via chalcone-based N-formyl-pyrazolines is described. N-Formyl-pyrazolines were prepared in excellent yield (81–96%) by the reaction of chalcones with hydrazine hydrate in the presence of formic acid, which undergoes intramolecular Friedel–Crafts acylation in the presence of trifluoroacetic acid (TFA) as a catalyst to afford functionalized 2-(substituted phenyl)-3,3a-dihydro-8H-pyrazolo[5,1-a]isoindol-8-ones in good to excellent yield (74–94%) at reflux in acetonitrile. Our synthetic route avoids expensive reagents and significantly improves yields. 相似文献
18.
Yevgen Posokhov Konstantin SytnikKasim Ocakoglu Mahmut Ku? Siddik Içli 《Journal of photochemistry and photobiology. A, Chemistry》2012,227(1):25-31
Spectral-luminescent properties of the newly synthesized 2-(3′-coumarinyl)-5-(2′-(R-amino)-phenyl)-1,3,4-oxadiazoles has been investigated in solvents of various polarity and hydrogen-bonding ability. It has been found that for all the studied compounds no excited state intramolecular proton transfer occurs despite the presence of coumarinyl fragment - electron acceptor effect of the coumarinyl fragment is not sufficient to increase the excited state acidity of the amino group. It has been found that the absorption spectra of the studied compounds shift to higher energy with increase in solvent polarity, whereas corresponding fluorescence spectra shift to lower energy with solvent polarity increase. It has been suggested that long-wavelength shifts of the fluorescence spectra of the studied compounds with increase in solvent polarity is caused by the solvent relaxation. The observed solvent relaxation effect allow us to propose some of the studied compounds as potential probes to monitor changes in solvent relaxation in low-polar media and as potential probes for rigidochromic effect. 相似文献
19.
20.
以2-氨基-5-取代苯氧甲基-1,3,4-噻二唑(1)为起始原料, 合成了中间体2-氯乙酰氨基-5-取代苯氧甲基-1,3,4-噻二唑)-2-乙酰亚胺(2)和2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-4-噻唑啉酮(3), 化合物3进一步与取代苯甲醛发生类Knoevenagle缩合反应, 得到了一系列2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-5-(取代苯基亚甲基)-4-噻唑啉酮类化合物4a~4p. 目标化合物4a~4p的结构经IR, 1H NMR和元素分析确证. 相似文献