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1.
J. C. Van De Grampel A. A. Van Der Huizen A. P. Jekel J. W. Rusch T. Wilting W. Akkerman 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-3):337-340
Abstract The partial aziridinolysis of (NPCl2)3,4 and (NPCl2)2 NSOCl yields non-geminal and geminal chloro-aziridinyl derivatives. Compounds N3P3Az6-nRn (R[dbnd]amino, alkoxy, aryloxy, id.) show in vitro and in vivo cytostatic activity. Structure-activity relationships are proposed. Phase I clinical trials of (NPAz2)2 NSOAz (Az[dbnd]1-aziridinyl) are summarized. 相似文献
2.
Hisanori Sugiura Yoshiaki Saklrai Yoshihide Masuda Hitoshi Takeda Shigekazu Kusabayashi Shunsuke Takenaka 《Liquid crystals》2013,40(3):441-450
Abstract The thermal properties of 4-octyloxyphenyl 4-(4-R-3-nitrobenzoyloxy) benzo-ates (1) and 4-(4-octyloxybenzoyloxy)phenyl 4-R-3-nitrobenzoates (2) have been examined, where R = hydrogen, halogens, alkyl and alkoxy groups. The derivatives of compound 1 incorporating hydrogen, halogens, methoxy and nitro groups show a smectic A phase having a bilayer arrangement, and the others with a long alkoxy group show the SA phase with the monolayer arrangement. The derivatives of compound 2 incorporating halogens, and the nitro group show the SA phase with the monolayer arrangement. The alkoxy derivatives show a smectic C phase as well as the nematic phase. The nitro group at the lateral position tends to increase the ratio of the SA-N transition temperature to the N-I. The effect of the nitro group on the smectic properties has been discussed in terms of the structural and electrostatic nature of the nitro group. 相似文献
3.
Abstract We have introduced an oxygen atom and a carbon-carbon double bond with a trans-configuration (E) into the terminal alkyl chain of a wide variety of liquid crystalline cyclohexane derivatives to produce a variety of new methyl (E)-allyl ethers. The melting points and tendency to form smectic mesophases are often low, while nearly all of the compounds prepared exhibit a nematic phase. Thus, even two-ring derivatives can exhibit nematic phases over a wide temperature range (≤80°C), sometimes starting below room temperature (T m≈10°C). Comparisons with the corresponding derivatives incorporating either just an oxygen atom or just a carbon-carbon double bond in the same position indicate that synergetic effects lead to broader nematic phases than would otherwise have been expected. Thus many of the new methyl (E)-allyl ethers exhibit nematic phases over a wider temperature range than the corresponding materials with an unsubstituted alkyl chain attached to the cyclohexyl ring. The new compounds are easily prepared from known starting materials. Many intermediates are themselves liquid crystalline. This allows investigation of the relationship between liquid crystal transition temperatures and the nature of the terminally substituted alkyl chain (for example, incorporating C[dbnd]C, OH, CO2C2H5 and OCH3 groups). 相似文献
4.
In this study, we synthesized a new series of substituted aliphatic 1,3,4-thiadiazol-2(3H)-one derivatives (6-24) in yields ranging from 42 to 70% with an interesting mechanism that involves internal nucleophilic substitution followed by an SN2-type nucleophilic substitution. First, 1-(4-chlorophenyl)-2-((5-methyl-1,3,4-thiadiazol-2-yl)thio)ethanone (3) was synthesized from the reaction of 5-methyl-1,3,4-thiadiazole-2-thiol (1) with 2-bromo-1-(4-chlorophenyl)ethanone (2) in the presence of potassium hydroxide. Then, 1-(4-chlorophenyl)-2-((5-methyl-1,3,4-thiadiazol-2-yl)thio)ethanol (4) was synthesized by a reduction reaction of this compound using NaBH4. Finally, 5-methyl-3-alkyl-1,3,4-thiadiazol-2(3H)-one derivatives (6-24), which are the target compounds, were synthesized from the reaction of this compound (4), which is a secondary alcohol with various alkyl halides (5a-n) in the presence of sodium hydride (NaH). This study presents an interesting reaction mechanism related to the synthesis of aliphatic 1,3,4-thiadiazol-2(3H)-one derivatives that is not recorded in the literature. 相似文献
5.
N. A. Buina G. M. Husnullina I. A. Vuretdinov A. E. Arbuzov 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4)
Abstract This communication deals with a simple method for preparation of X-phosphorylated sugars by the reaction of trivalent phosphorus derivatives with 1-α,β-azides of 2,3,4,5-tetraacetylated and 2,3,4,6-tetra(trimethyl)silylated glycose. It has been established that ohosphimine derivatives, obtained as a result of the Staudinger reaction, can be easily hydrolyzed to give derivatives of acetylated glucosaminphosphoric acids. It has been discovered that susceptibility to hydrolysis depends on the phosphorus suhstituents. When using esters of trivalent phosphorus the rate of hydrolysis for compounds with alkyl substituents decreases in order C3H7 > C2H5O >> CH3O This can probably be explained by the electronic and steric influence of the alkyl groups. 相似文献
6.
Issa Yavari Jamil Sheykhahmadi Hamed Saffarian Nooshin Zahedi Samira Bahemmat Mohammad Reza Halvagar 《合成通讯》2013,43(19):2608-2614
AbstractThe four-component reaction among arylhydrazine, alkyl acetoacetate derivatives, alkyl isocyanides, and dialkyl acetylenedicarboxylates, leading to the formation of dialkyl 2-[(Z)-(alkylamino)(3-alkyl-5-oxo-1-phenyl-1,5-dihydro-4H-pyrazol-4-ylidene)methyl] fumarates is described. The structure of target compounds was confirmed using X-ray diffraction study. These pyrazolone derivatives contain a highly twisted exocyclic 1,3-butadiene moiety with skew (??=?87°) geometry. 相似文献
7.
Ülkü Yılmaz Hasan Küçükbay 《Phosphorus, sulfur, and silicon and the related elements》2020,195(7):580-585
AbstractN-heterocyclic carbene (compound b) was synthesized from reaction of 1-(3-phenylpropyl)-3-methylbenzimidazolium iodide (a) and a strong base in an argon atmosphere. Then, 1-(3-phenylpropyl)-3-methylbenzimidazolium-2-carbodithioate (c) was prepared with carbene and CS2. Finally, a group of alkyl 1-(3-phenylpropyl)-3-methylbenzimidazolium-2-carbodithioate halides was synthesized with alkyl halides and compound c, occurring products 1-6. Structural characterization of compounds was performed 1H, and 13C NMR, IR, and MS spectroscopy and elemental analysis. 相似文献
8.
Rudolph Francke Gerd-Volker Röschenthaler 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3-4)
Abstract The reactions of dihaloaminophosphines RNHPF2, (R=H, Me, tBu) and R2NPCl2 (R?Me, Et, SiMe3; R2?CH2(CH2CMe2)2 with LiOCH(CF3)2 yield the corresponding aminophosphites R2NP[OCH(CF3)2)2. Hexafluoroacetone reacts with RNH[OCH(CF3)2]2 as well as MeNHPF2 and tBuNHPF2 in good yields to the 1,3,5λ5-oxazaphosphetanes 1-4, which show rapid pseudorotation at room temperature. 相似文献
9.
Steven M. Schultz Gerald Kehr Roland Fröhlich Gerhard Erker Nadia Kapernaum Constanze Hägele 《Liquid crystals》2013,40(8):919-926
A series of 2‐(4‐n‐alkylphenyl)indenes (3) with different alkyl substituents (CH3 to C10H21) were synthesized and systematically characterized using differential scanning calorimetry, polarizing optical microscopy and X‐ray diffraction compared with 2‐phenylindene (3a). Depending on the alkyl chain length, highly ordered crystal‐smectic E mesophases were observed and confirmed by X‐ray diffraction for the derivatives 3h–3k with heptyl to decyl chains (n = 6?9). For 3f with a pentyl side chain (n = 4), an X‐ray crystal structure analysis was carried out. 相似文献
10.
《Analytical letters》2012,45(4):219-222
Abstract The polarographic reduction of gem-halogeno-nitro derivatives has been studied in an aprotic organic medium. The electrochemical reduction of derivatives of the type (CH3)2 CXNO2 (where X=Br, Cl, H) leads to the 2, 3-dimethyl 2, 3 dinitrobutane with a good yield. 相似文献
11.
Abstract The reaction of acetonitrile with PCl, results in the ionic compounds (1) to (4) containing the trichloro[2-chloro-2-[(trichlorophosphoranyli-dene)amino]ethenyl]phosphorus cations and not in the compounds [CH2?C?NPCl3]PCl61 or trichloro[2-chloro-1 -[(trichlorophosphoranyli-dene)amino] ethenyl]phosphorus hexachlorophosphate (5) as assumed from 31P-NMR spectra [2, 3]. The crystal structures of the compounds (1) to (4) were determined with X-rays at 95K. As observed for the CI-C(NPCl3); cation all the cations show cis-trans conformations with respect to their CI-C-X-P torsion angles. The wcl3 groups of the cations have two different orientations with one C?N?P?CI torsion angle of about 0° (cis) as in (1) or about 180° (trans) as in (3) and (4). In the salt (2) there are two formula units in the asymmetric unit with one cation showing the cis and the other showing the tram conformation. 相似文献
12.
Structural parameters of the cation [C(NPCl3)3]+ in vacuum and in acetonitrile are calculated by the methods RHF/6-311G(3d6), RHF/6-31(3d5) and B3LYP/6-311(3d5f7). Formation energy of the free adduct (MeCN) 2[C(NPCl3)3]+ is calculated and nonspecific character of interaction of the cation with liquid acetonitrile is established. Vibration spectrum of the cation is calculated and theoretical interpretation of IR and Raman spectra of the salt [C(NPCl3)3]+[SbCl6]? is refined. 相似文献
13.
Using (NPCl2)3 as a reagent for Bischler-Napieralski ring closure, various β-aryl amides were converted to 3,4-dihydroisoquino line derivatives. 相似文献
14.
An efficient route to the synthesis of 1,3-dienylphosphonates (1) has been developed for the first time by the substitution of propargylic esters (2) to the diethyl phosphite (3) nucleophile in the presence of Pd2(dba)3 · CHCl3 (2 mol %) and 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (4 mol%). Both the alkyl and aryl 1,3-dienylphosphonates can be prepared from this transformation. Supplemental materials are available for this article. Go to the publisher's online edition of Synthetic Communications® to view the free supplemental file. 相似文献
15.
Prof. Dr. Richard Neidlein Wolf-Dieter Ober 《Monatshefte für Chemie / Chemical Monthly》1976,107(5):1251-1258
The -isothiocyanato-ketone 1 reacts with substituted hydrazines (2) in alkaline solution to form 2-alkyl-5,6-dihydro-(2H)-1,2,4-triazepine-3(4H)-thiones (3); the intermediate thiosemicarbazide derivatives (6), formed by addition of the hydrazine derivatives to the isothiocyanate group, could be isolated. CH3I and BrCH2COOC2H5 alkylate3 at sulfur, and the fusedring compounds14 and16 were isolated.
Herrn Prof. Dr. Dr. h. c.K. E. Schulte zum 65. Geburtstag gewidmet.
Dissertation 1976, Universität Heidelberg.
R. Neidlein undW. D. Ober, Mh. Chem.107, 1241 (1976). 相似文献
Herrn Prof. Dr. Dr. h. c.K. E. Schulte zum 65. Geburtstag gewidmet.
Dissertation 1976, Universität Heidelberg.
R. Neidlein undW. D. Ober, Mh. Chem.107, 1241 (1976). 相似文献
16.
《Analytical letters》2012,45(19):1539-1548
Abstract A HPLC method for the separation of phenol derivatives has been developed either on a RP Phenyl-bonded or an alkyl C18 -bonded columns. Derivatization with diazotized sulphanilic acid allows a reversed-phase chromatography with spectrophotometric detection at 370 nm. The method sensitivity permits detection down to 0.08- 0.15 ng of phenols. In particular structure-retention time relationships are discussed. 相似文献
17.
Maw-Ling Wang Ho-Sheng Wu 《Journal of polymer science. Part A, Polymer chemistry》1992,30(7):1393-1399
The ion-exchange rate limitation on the kinetics of the series substitution reactions between hexachlorocyclotriphosphazene (NPCl2)3 and 2,2,2-trifluoroethanol (HOCH2CF3) by polystyrene-bound tri-n-butylammonium ion in an organic solvent/alkaline solution was studied. It was found that the diffusional limitation involves both ion diffusion and organic reactant diffusion within the catalyst pellet. The displacement reaction rate of (NPCl2)3 in the organic phase was limited by the particle diffusion and the intrinsic reactivity together. The film diffusion in the bulk solution limited the rate of ion exchange. The mass transport of the ion-exchange step in the aqueous phase was not improved by increasing the concentration of NaOCH2CF3. Drastic kinetic rate improvement was achieved with proper adjustment of the volume of the aqueous solution which was a low concentration of salt in the aqueous phase. 相似文献
18.
F. Asinger D. Neuray E. Wilms A. Saus 《Monatshefte für Chemie / Chemical Monthly》1973,104(1):137-154
Zusammenfassung Die Oxydation des 2-Methyl-3-äthylthiomorpholins (1) bzw. seines Hydrochlorids (1·HCl) mit 30proz. H2O2 liefert bei 0°C 87 bzw. 84% 2-Methyl-3-äthylthiomorpholin-1-oxid (4), bei 50°C 41 bzw. 46% 2-Methyl-3-äthylthiomorpholin-1,1-dioxid (7). Aus 2-Methyl-3-äthyl-4-formylthiomorpholin (2) bzw. 2-Methyl-3-äthyl-4-acetylthiomorpholin (3) erhält man die entspr. Sulfoxide (5 83%] bzw.6 [80%]), wenn man mit 30proz. H2O2 bei 0°C in Wasser bzw. Eisessig oxydiert, dagegen die entspr. Sulfone (8 [93%] bzw.9 [73%]), wenn in Ameisensäure bzw. Eisessig mit überschüss. 85proz. H2O2 bei 100°C oxydiert wird.8 und9 lassen sich mit verd. HCl glatt (ca. 90%) zu7 verseifen.Auf Basis von4 und7 werden zahlreiche s-Triazin-Derivate (10–26) und durch Addition von4 und7 an Isocyanate und Senföle einige Harnstoff- (27–31, 35–38) und Thioharnstoff-Derivate (32–34) dargestellt.
1. Mitt.:F. Asinger, H. Offermanns, A. Saus, C. Dudeck, D. Neuray undE. Wilms, Mh. Chem.104, 118 (1973).
80. Mitt.:F. Asinger, A. Saus undD. Neuray, Ann. Chem. (im Druck).
Teil der DiplomarbeitE. Wilms, Techn. Hochschule Aachen, 1969; Teil der DissertationE. Wilms, Techn. Hochschule Aachen 1971. 相似文献
On the reactivity of alkyl substituted thiomorpholines, II1 (Joint action of elemental sulfur and gaseous ammonia upon ketones, LXXXI2)
Oxidation of 2-methyl-3-ethyl-thiomorpholine (1) and the corresponding hydrochloride (1·HCl) with 30% H2O2 leads to the 2-methyl-3-ethyl-thiomorpholine-1-oxide (4) at 0°C in a yield of 87 and 84%, resp.; at 50°C 2-methyl-3-ethyl-thiomorpholine-1.1-dioxide (7) is formed in a yield of 41 and 46%, resp. By oxidation of 2-methyl-3-ethyl-4-formyl-thiomorpholine (2) and 2-methyl-3-ethyl-4-acetyl-thiomorpholine (3) with a 30% solution of H2O2 at 0°C in water or acetic acid, resp., the corresponding sulfoxides (5 [83%] and6 [80%]) are obtained; with an excess of 85% H2O2 in formic or acetic acid at 100°C the respective sulfones (8 [93%] and9 [73%]) are formed.8 and9 are easily saponified with dilute HCl to7 in a yield of about 90%.A large number of s-triazine derivatives (10–26) are prepared from4 and7; by addition of isocyanates and thio isocyanates to4 and7 urea- (27–31, 35–38) and thiourea derivatives (32–34) are obtained.
1. Mitt.:F. Asinger, H. Offermanns, A. Saus, C. Dudeck, D. Neuray undE. Wilms, Mh. Chem.104, 118 (1973).
80. Mitt.:F. Asinger, A. Saus undD. Neuray, Ann. Chem. (im Druck).
Teil der DiplomarbeitE. Wilms, Techn. Hochschule Aachen, 1969; Teil der DissertationE. Wilms, Techn. Hochschule Aachen 1971. 相似文献
19.
İsa Karaman Hayreddin Gezegen Mustafa Ceylan Merve Dilmaç 《Phosphorus, sulfur, and silicon and the related elements》2013,188(5):580-586
Abstract In this study, a series of novel β-mercapto carbonyl derivatives (3a–j) was prepared by addition of thiophenol (2) to chalcones (1a–j) in the presence of catalytic amount of iodine (10 mol%) in CH2Cl2. Antibacterial and antifungal in vitro properties of the synthesized compounds were tested against some human pathogenic microorganisms by employing the disk diffusion technique. For the most active compounds, also minimum inhibitory concentrations (MICs) were determined. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. 相似文献
20.
Zusammenfassung Durch Nitrieren des Indandion-Analogons1 mit konz. HNO3 wurde das Mononitroderivat (2b) in sehr guter Ausbeute gewonnen, in dem das H-Atom in der Methingruppe des 7 gliedrigen Diketonringes durch die Nitrogruppe substituiert ist. Bei Reduktion des Mononitroderivats geht dieses in ein Aminoderivat mit dimerer Struktur (7) über. Aus den Halogenderivaten von1 wurde durch Ersetzen des Halogens gegen die Aminogruppe das entsprechende Ketimidoderivat (5) gewonnen.
Mit 1 Abbildung
4. Mitt.:B. Aleksiev undM. Miloev 1. 相似文献
Preparation of new indandione analogues, V.: Nitro and amino derivatives of the indandione analogue from diphenic anhydride and phenylacetic acid
The nitration of the indandione analogue1 with conc. HNO3 afforded a mononitro derivative (2b) in very good yield, the nitro group substituting the H atom in the methine group of the 7membered diketone ring. Upon reduction this nitro compound gave a dimeric amino derivative (7). When the halogenated derivatives of1 were treated with NH3 in order to replace the halogen by an amino group, a ketimino derivative (5) was isolated.
Mit 1 Abbildung
4. Mitt.:B. Aleksiev undM. Miloev 1. 相似文献