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1.
Zusammenfassung In Fortsetzung unserer Synthesen wurden aus p-Amino-benzoesäure, ihrem Äthylester, p-aminoacetophenon und Sulfanilamid die entsprechenden Arylhydrazono-cyanacetylcarbamid-säureäthylester (1 a–1 d), 1-Aryl-6-azauracil-5-carbonsäure-nitrile (2 a–2 d), 1-Aryl-6-azauracil-5-carbonsäure (3 a–3 d) und die Thioamide (4 a–4 d) dieser Säuren hergestellt. Durch Decarboxylierung der Säure3 a wurde 1-(p-Carboxyphenyl)-6-azauracil (5 a) gewonnen.
From p-aminobenzoic acid, its ethyl ester, p-aminoaceto-phenone and sulfanilamide the corresponding ethyl arylhydrazonocyanoacetylcarbamidates (1a–1 d), 1-aryl-6-azauracil-5-carboxylic acid nitriles (2 a–2 d), carboxylic acids (3 a–3 d) and thioamides (4 a–4 d) have been prepared. Decarboxylation of3 a yielded 1-(p-carboxyphenyl)-6-azauracil (5 a).


7. Mitt.:J. Slouka undP. Pe, Mh. Chem.98, 1201 (1967).  相似文献   

2.
5-Alkyl-5,6-dihydrobenzimidazo[2,1 -h]pteridine-2,4(1H,3H)-diones (4 a–d) have been synthesised by the condensation of 2-(alkyl-aminomethyl)benzimidazole dihydrochloride (1 a–d) with 5-bromobarbituric acid (2). Similarly, 5-alkyl-5,6-dihydro-4 a-nitrobenzimidazo[2,1 -h] pteridine-2,4(3H,4aH)-diones (10 a–d) have also been synthesised by the condensation of1 a–d with 5-bromo-5-nitrobarbituric acid (8) followed by cyclisation of the intermediate 5-[(benzimidazol-2-ylmethyl)alkylamino]-5-nitrobarbituric acid (9 a–d) with 5% NaOH. Thermal cyclisation of the intermediates9 a–d have also been studied. Methylation of the compound10 a has been carried out with CH3I and K2CO3 usingD M F as solvent to confirm cyclisation. The structures are supported by elemental analyses, IR and PMR spectra.
Substituierte Benzimidazo[2,1 -h]pteridin-2,4-dione
Zusammenfassung Die 5-Alkyl-5,6-dihydrobenzimidazo[2,1 -h]pteridin-2,4(1H,3H)-dione4 a-d wurden mittels Kondensation von 2-(Alkylaminomethyl)benzimidazolidhydrochloriden1 a–d mit 5-Brombarbitursäure (2) dargestellt. In ähnlicher Weise wurden die 5-Alkyl-5,6-dihydro-4a-nitrobenzimidazo[2,1 -h]pteridin-2,4(3H,4aH)-dione10 a–d über die Kondensation von1 a–d mit 5-Brom-5-nitrobarbitursäure (8) und nachfolgender Cyclisierung der intermediären 5-[(Benzimidazol-2-ylmethyl)alkylamino]-5-nitrobarbitursäuren9 a–d mit 5% NaOH dargestellt. Die thermische Cyclisierung der Produkte9 a–d wurde ebenfalls untersucht. Die Verbindungen wurden mittels Elementaranalyse, IR und PMR charakterisiert.
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3.
Reaction of ethoxymethylene-malonitrile and ethoxymethyleneethyl cyanoacetate, resp., with 4-hydroxy-2-pyridones (1a–b) and 4-hydroxy-2-quinolones (3a–b) leads to 2,5-dioxo-5,6-dihydro-2 H-pyrano[3,2-c]pyridine-(2a–d) and 2,5-dioxo-5,6-dihydro-pyrano[3.2-c]quinoline-derivatives (4a–d), resp.2a–d and4a–d exhibit remarkable visible fluorescence. Absorption- and emmission-data in different solvents are reported.  相似文献   

4.
Zusammenfassung Die Darstellung einigerMannichbasen (3 a-f) bzw.Mannich-basen-hydrochloride (2 a-f) und zahlreicher s-Triazin-Derivate (4 a-d, 5 a–m, 6 a–w, 7 a–e, 8 a–d, und9 a–l) auf Basis des unsubstituierten Thiomorpholins (1 a) sowie C-mono-[2-Methylthiomorpholin (1 b) und 2-Äthylthiomorpholin (1 c)] und C-dialkylierter Thiomorpholine [2-Methyl-3-äthylthiomorpholin (1 d)] wird beschrieben.
Concomitant action of elementary sulfur and gaseous ammonia upon ketones, LXXIX: On the reactivity of alkyl substituted thiomorpholines, I
The preparation of someMannichbases (3 a-f) andMannich base hydrochlorides (2 a-f), resp., and numerous s-triazine derivatives (4 a-d, 5 a–m, 6 a–w, 7 a–e, 8 a–d, and9 a–l) based upon unsubstituted thiomorpholine (1 a) as well as C-mono-[2-methylthiomorpholine (1 b) and 2-ethylthio-morpholine (1 c)] and C-dialkylated thiomorpholines [2-methyl-3-ethylthiomorpholine (1 d)] is described.


HerrE. Wilms dankt der Deutschen Texaco AG. für die Gewährung eines Stipendiums herzlichst.  相似文献   

5.
The reaction of dimeric rhodium precursor [Rh(CO)2Cl]2 with two molar equivalent of 1,1,1-tris(diphenylphosphinomethyl)ethane trichalcogenide ligands, [CH3C(CH2P(X)Ph2)3](L), where X = O(a), S(b) and Se(c) affords the complexes of the type [Rh(CO)2Cl(L)] (1a–1c). The complexes 1a–1c have been characterized by elemental analyses, mass spectrometry, IR and NMR (1H, 31P and 13C) spectroscopy and the ligands a–c are structurally determined by single crystal X-ray diffraction. 1a–1c undergo oxidative addition (OA) reactions with different electrophiles such as CH3I, C2H5I and C6H5CH2Cl to give Rh(III) complexes of the types [Rh(CO)(COR)ClXL] {R = –CH3 (2a–2c), –C2H5 (3a–3c); X = I and R = –CH2C6H5 (4a–4c); X = Cl}. Kinetic data for the reaction of a–c with CH3I indicate a first-order reaction. The catalytic activity of 1a–1c for the carbonylation of methanol to acetic acid and its ester is evaluated and a higher turn over number (TON = 1564–1723) is obtained compared to that of the well-known commercial species [Rh(CO)2I2] (TON = 1000) under the reaction conditions: temperature 130 ± 2 °C, pressure 30 ± 2 bar and time 1 h.  相似文献   

6.
Electrochemical oxidation of catechol (1a), 3-methylcatechol (1b) and 3-methoxycatechol (1c) in the presence of 1,3-diethyl-2-thiobarbituric acid (3) as a nucleophile in aqueous solution has been studied using cyclic voltammetry and controlled-potential coulometry. The results indicate that (1a1c) participating in a 1,4 (Michael) addition reaction converts to dispirothiopyrimidine derivatives (6a6c). The electrochemical synthesis of 6a6c has been successfully performed in an undivided cell in good yield and purity.  相似文献   

7.
Summary Photolysis of 3-phenylpropiophenones1 a–d in the presence of 2,4,6-triphenylpyrylium tetrafluoroborate (TPT) yields the corresponding ,-unsaturated ketones2 a–c and1 d (from1 c), together with acetophenone (3), benzophenone (4), benzoic acid (5) and benzaldehyde (6), presumably by fragmentations of the radical cation1 + ·, generated via a single electron transfer process from1 to the excitedTPT.
Photofragmentierung von 3-Phenylpropiophenonen via Elektronenübertragung
Zusammenfassung Photolyse der 3-Phenylpropiophenone1 a–d in Gegenwart von 2,4,6-Triphenyl-pyrylium-tetrafluoroborat (TPT) ergeben die entsprechenden ,-ungesättigten Ketone2 a–c und1 d (aus1 c), neben Acetophenon (3), Benzophenon (4), Benzoesäure (5) und Benzaldehyd (6), vermutlich durch Fragmentierung des Radikal-Kations1 + ·, das mittels Übertragung eines Elektrons von1 zuTPT im angeregten Zustand erzeugt wird.
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8.
A series of new 1-(alkenoyl/hydroxyalkenoyl)-4-benzoyl-thiosemicarbazides 2a-d and 2-benzamide-5-alkenyl/hydroxyalk- enyl-1,3,4-thiadiazoles 3a-d were synthesized from fatty acid hydrazides. Structure of all these compounds was confirmed by IR, IH NMR, Sac NMR, mass spectra and elemental analysis. The bioassay results indicate that some compounds 2e, 2d, 3e and 3d have good antibacterial activity.  相似文献   

9.
Summary Treatment of 2-phenoxypropionic acid with polyphosphoric acid gave substituted benzofuran-3-ones (2a–h), which were converted into 2,3,4-trihydrodibenzofuran-3-ones (4a–h)via the compounds3a–h.Clemmensen reduction of the compounds4a–h gave the 2,3,4-trihydrodibenzofuranes (5a–h).
Eine einfache Synthese von 2,3,4-Trihydrobenzofuranen
Zusammenfassung Behandlung von 2-Phenoxypropionsäure mit Polyphosphorsäure lieferte die substituierten Benzofuran-3-one (2a–h), welche über3a–h in die 2,3,4-Trihydrodibenzofuran-3-one (4a–h) übergeführt wurden. DurchClemmensen-Reduktion von4a–h wurden die gewünschten 2,3,4-Trihydrobenzofurane (5a–h) erhalten.
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10.
Some 5H-pyrimido[4,5-e](1,2,4)-triazolo[3,4-b](1,3,4)-thiadiazine-7,9-(6H,8H)-diones (4 a–d) have been synthesised by the condensation of 3-alkyl-4-amino-5-mercapto-(1,2,4)-triazoles (1 a–d) with 5-bromobarbituric acid (2a). Similarly some 9a-nitro-5H-pyrimido[4,5-e](1,2,4)-triazolo[3,4-b](1,3,4)-thiadiazine-7,9(8H,9aH)-diones (5 a–d) have been obtained by the condensation of1 a–d with 5-bromo-5-nitrobarbituric acid (2b) and final cyclisation withPPA. The structures have been confirmed by PMR spectra and analytical results.
Pyrimido[4,5-e](1,2,4)-triazolo[3,4-b](1,3,4)-thiadiazin-7,9(6H,8H)-dione
Zusammenfassung Es wurden einige 5H-pyrimido[4,5-e](1,2,4)-triazolo[3,4-b](1,3,4)-thiadiazin-7,9(6H,8H)-dione (4 a–d) mittels Kondensation von 3-Alkyl-4-amino-5-mercapto-(1,2,4)-triazolen (1 a–d) mit 5-Brombarbitursäure (2 a) dargestellt. Des weiteren wurden einige 9a-Nitro-5H-pyrimido[4,5-e](1,2,4)-triazolo[3,4-b](1,3,4)-thiadiazin-7,9(8H,9aH)-dione (5 a–d) über die Kondensation von1 a–d mit 5-Brom-5-nitrobarbitursäure (2 b) und anschließender Cyclisierung mitPPA synthetisiert. Die angeführten Strukturen wurden mittels PMR-Spektren und analytischen Daten abgesichert.
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11.
Summary Several 7-methyl-5-alkyl-2-vinylpyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-diones were prepared. The successful cyclization and alkylation of 6-(-methylbenzylidenehydrazino)-1-methyluracils2a–d using dimethylformamide acetals at high temperature provided6a–d,7a–d, and8a–d. Treatment of6a–d and7a–d with acid afforded 7-methyl-5-alkylpyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-diones9a,b; under the same conditions,3a–d reacted to 7-methylpyrazolo[3,4-d]-pyrimidine-4,6(5H)-dione (4) in good yield.
DMF-Acetale als Alkylierungs- und Ringschlußreagentien: ein einfacher Weg zu substituierten Pyrazolo[3,4-d]pyrimidin-4,6(5H,7H)-dionen
Zusammenfassung Es wurden verschiedene 7-Methyl-5-alkyl-2-vinylpyrazolo[3,4-d]pyrimidin-4,6(5H,7H)-dione hergestellt. Cyclisierung und Alkylierung der 6-(-Methylbenzylidenhydrazino)-1-methyl-uracile2a–d mit Hilfe von Dimethylformamidacetalen bei hohen Temperaturen ergab6a–d,7a–d und8a–d. Behandlung von6a–d und7a–d mit Säure lieferte die 7-Methyl-5-alkylpyrazolo[3,4-d]pyrimidin-4,6(5H,7H)-dione9a,b; unter den gleichen Bedingungen reagierten3a–d in guter Ausbeute zu 7-Methylpyrazolo[3,4-d]pyrimidin-4,6(5H)-dion (4).
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12.
Summary The synthesis of some 5-cyano-4-hydroxy-2-pyridone derivatives (3 a–c) by condensation of 3-aminocrotononitrile (1) with substituted diethylmalonates (2 a–c) is described. Reaction of3 a with phosphorus oxychloride yields 4,6-dichloro-3-pyridinecarbonitrile (7 a), which reacts with various nucleophiles to give substituted 3-pyridinecarbonitriles (8–10).See ref. [1]  相似文献   

13.
8-G-1-(p-YC6H4CCSe)C10H6 [2 (G = Cl) and 3 (G = Br): Y = H (a), OMe (b), Me (c), F (d), Cl (e), CN (f) and NO2 (g)] have been prepared and the NMR spectra measured, in addition to 1 (G = H). Structures have been determined by X-ray crystallographic analysis for 2b, 2e and 2g, which are all type B (B), where the Se–Csp bond is placed in the naphthyl plane in B. The type is classified as A if the Se–Csp bond is perpendicular to the naphthyl plane. Structures around the p-YC6H4 (Ar) group are pd (perpendicular) for Y = OMe (2b) and Cl (2e) and pl (planar) for Y = NO2 (2g), where the Se–CNap bond is placed in the aryl plane in pl and perpendicular to the plane in pd. The 1b (A: pd) structure changes dramatically on going to 2b (B: pd) with G = Cl at the 8-position. The effect is called the G-dependence in 2. The G-dependence arises from the energy lowering effect of the np(Cl)σ*(Se–Csp) 3c–4e interaction. Structures are both (B: pd) for 1e and 2e and both (B: pl) for 1g and 2g. One may realize that the structures are unchanged by G = Cl in place of G = H for Y = Cl and NO2 at a first glance. However, the B structures in 2e and 2g must be much more stabilized by the G-dependence of the np(Cl)σ*(Se–Csp) 3c–4e interaction or the GSe–Csp–Csp–Csp2 5c–6e type interaction. The structures of 2 and 3 are examined in solution based on the NMR parameters. The results show that 2 and 3 behave very similarly to each other and the structures are predominantly B, with some equilibrium between pd and pl around the aryl groups in solution. Quantum chemical calculations support the observations.  相似文献   

14.
Six new optically active poly(amide-imide)s(5a-f) were synthesized through the direct polycondensation reaction of N,N'-(4,4'- diphthaloyl)-bis-L-leucine(3) with six hydantoin derivatives(4a-f).Triphenyl phosphite(TPP)/pyridine in the presence of calcium chloride(CaCl_2) and N-methyl-2-pyrrolidone(NMP) were successfully applied for direct polycondensation.The polycondensation reactions produce a series of new poly(amide-imide)s(5a-f) in high yields,and inherent viscosity between 0.42 and 0.55 dL/g.The re...  相似文献   

15.
The synthesis of a new series of six-membered N,N′-diarylsubstituted methylene-bis-dihydro-2H-1,3-benzoxazines (5a-e) was achieved in excellent yields by Mannich-type condensation of N,N′-diarylsubstituted methylene-bis-o-hydroxybenzyl amines (4a- e) with formaldehyde in chloroform at reflux. These amines (4a-e) were obtained by the reduction of N, Nr-diarylsubstituted methylene-bis-o-hydroxybenzyl imines (3a-e) with NaBH4, which inturn were obtained by the condensation of methylene-bissalicylaldehyde (2) with various substituted arylamines.  相似文献   

16.
1,1-Dichloro-2-alkynes R1CCCHCl2 (4a–g; R1=Me, n-Pr, c-Pr, t-Bu, Ad, Nor, Ph) were synthesized with yields of 50–75% by chlorination with PCl5 of formylacetylenes (3a–g), prepared by oxidation of propargyl alcohols (1a–d) with CrO3·Py·HCl complex or acidolysis of propargyl acetals (2a–c) in the presence of catalytic quantities of pyridine; the corresponding alkynylchlorocarbenes, R1CCCCl (5a–g) were generated from them with powdered KOH in a two-phase system or t-BuOK. The latter were trapped by olefins with formation of 1-chloro-1-alkynylcyclopropanes (6a–t) with yields of up to 90%.See [1] for Communication 1.N. D. Zelinskii Institute of Organic Chemistry, Russian Academy of Sciences, 117913 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 5, pp. 1128–1135, May, 1992.  相似文献   

17.
Partial O-alkylation of 1,3:2,4-di-O-ethylidene-D-glucitol (1a), 1,2-O-isopropylidene-3-O-methyl--D-glucofuranose (1b), andR-(+)-1-O-benzylglycerol (1c) with benzyl chloride in a KOH/DMSO system results in products of monoalkylation at the secondary (4a–c) and at the primary hydroxyl (2a–c) in ratios of over 955 (a), 21 (b), and 11 (c), whereas (±)propane-1,2-diol (1d) gives only the product of 1-O-benzylation (2d). A qualitatively similar result is observed upon O-alkylation of diols (1a–e) with 2-methoxyethanol tosylate.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 776–781, April, 1993.  相似文献   

18.
A new, mild and friendly method for the synthesis of (N → B) phenyl[N-alkyliminodiacetate-O,O′,N]boranes 27 is reported. All compounds were identified by 1H, 11B, 13C NMR and their high resolution mass spectra (HRMS) are reported. The structure of the compounds 2, 4 and 5 were established by single crystal X-ray. Compounds 2 and 4 crystallized with two independent molecules 2A, 2B and 4A, 4B, respectively in the asymmetric unit. These molecular structures established the bicyclic structure showing a N → B bond length of 1.666 (2) Å for 2A, 1.675 (2) Å for 2B, 1.675 (3) Å for 4A, 1.663 (3) Å for 4B and 1.679 (2) Å for 5, as well as different torsion angles of the junction, 28.70 (2)° (C11–B1–N6–C17) for 2A, 21.50 (2)° (C11a–B1a–N6a–C17a) for 2B, 25.76 (0.26)° (C11–B1–N6–C17) for 4A, 21.96 (0.28)° (C11a–B1a–N6a–C17a) for 4B and −29.22 (0.20)° (C5–N1–B1–C13) for 5.  相似文献   

19.
Summary Oxazolin-2-ylidene-malononitriles3a–d, obtainable from thioketenaminals and -halogen-ketones, react with primary and secondary amines to afford 2,4-diamino-pyrroles5a–h. Mercaptobenzen as nucleophilic agent gives the 4-amino-2-phenylthio-pyrrole5j. Analogously, cyano-(3,5-diphenyl-3H-oxazol-2-ylidene)-acetic acid methyl esters were prepared as intermediates for the synthesis of 2-amino-4-oxo-pyrrolines10a–d. The isomeric 4-amino-2-oxo-pyrrolines13a–d can be obtained from 4-amino-2-methoxy-pyrroles, which serves as proof for the position of substituents. The structures were investigated by1H and13C NMR spectroscopy.
Neue Synthesen von 2,4-Diaminopyrrolen und Aminopyrrolinonen
Zusammenfassung Die Oxazolin-2-yliden-malononitrile3a–d. die aus Thioketenaminalen und -Halogenketonen erhalten wurden, reagieren mit primären und sekundären Aminen zu den 2,4-Diaminopyrrolen5a–h. Mercaptobenzol als nukleophiles Reagens liefert 4-Amino-2-phenylthiopyrrol (5j). Analog wurden Cyan-(3,5-diphenyl-3H-oxazol-2-yliden)-essigsäuremethylester als Zwischenprodukte für die Synthese der 2-Amino-4-oxo-pyrroline10a–d hergestellt. Die isomeren 4-Amino-2-oxo-pyrroline13a–d können aus den 4-Amino-2-methoxy-pyrrolen11a,b erhalten werden, was als Nachweis für die Position der Substituenten dient. Die Verbindungen wurden1H- und13C NMR-spektroskopisch untersucht.
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20.
Summary Reactions of 6-glycopyranosylaminopyrimidin-4-ones1 a–d with malonic, methyl malonic and ethyl malonic acids are discussed in this paper. These reactions have been carried out in acetic anhydride at 100°C affording the 8-glycopyranosylpyrido[2,3-d]pyrimidin-4-ones2 a–d,3 c–d and the 5-acyl-6-glycopyranosylaminopyrimidin-6-ones4 a–d,5 a–d.
Reaktion von 6-Glycopyranosylaminopyrimidin-4-onen mit Malonsäuren. Synthese von 8-Glycopyranosylpyrido[2,3-d]pyrimidin-4-on-Dervaten
Zusammenfassung Es werden Reaktionen der 6-Glycopyranosylaminopyrimidin-4-one1 a–d mit Malonsäure, Methylmalonsäure und Ethylmalonsäure diskutiert. Die Reaktionen wurden in Essigsäureanhydrid bei 100°C ausgeführt und ergaben 8-Glycopyranosylpyrido[2,3-d]pyrimidin-4-one2 a–d,3 c–d und die 5-Acyl-6-glycopyranosylaminopyrimidin-6-one4 a–d und5 a–d.
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