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1.
A Cyclic Methylenediphosphinic Acid: 1,3‐Dihydroxy‐1,3‐dioxo‐1,2,3,4‐tetrahydro‐1λ5,3λ5‐[1,3]diphosphinine Strong acids protonate 1,3‐bis(dimethylamino)‐1λ5,3λ5‐[1,3]diphosphinine ( 5 ) to give the corresponding cation. The protonation is followed by hydrolytic cleavage of the dimethylamino groups resulting in the formation of the cyclic methylenediphosphinic acid ( 6 ). 相似文献
2.
Stefan Plank Gernot Heckmann Wolfgang Schwarz Bernhard Neumüller Ekkehard Fluck 《无机化学与普通化学杂志》1999,625(10):1712-1720
Diphosphabenzenes. VI. New 1λ5, 3λ5-[1,3]Diphosphinines with Thio and Seleno Phosphonic Acid Groups – Preparation, Crystal Structure, NMR Data, and Coordination to PdII Preparation of N,N,N′,N′-tetraethyl-P-phenylethinyl phosphonothioacid diamide ( 2 ) and the corresponding phosphonoselenoacid diamide ( 3 ) are described. 2 and 3 react with 1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete ( 1 ) to yield 1λ5,3λ5-[1,3]diphosphinine derivatives 4 and 5 . With (bzl)2Cl2Pd 5 forms the coordination compound 6 . All new compounds 2–6 are characterized by their nmr and ir spectra, the structures of 4–6 are further elucidated by X-ray structural analyses. 相似文献
3.
Transition Metal Complexes of 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-Diphosphete 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3aλ5-diphosphete, 1 , reacts with W(CO)6 to yield the isomeric complexes {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)tungsten 4 and {1,1,3,3-tetrakis(dimethylamino)-1,4-dihydro-1λ5,3λ5-[1,3]diphosphetium}(pentacarbonyl)tungsten 5 . With Cr(CO)6 the complex {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)chromium 6 is formed. From the reaction products of Fe3(CO)12 and Fe2(CO)9 with 1 the complex {1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete}(pentacarbonyl)iron 7 could be isolated. Properties, nmr, ir and mass spectra of the new compounds are reported. 6 and 7 were characterized by X-ray structure determinations. 相似文献
4.
Fred Rosche Gernot Heckmann Ekkehard Fluck Bernhard Neumüller 《Heteroatom Chemistry》1996,7(5):341-347
1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1, reacts with diphenylchlorophosphane to yield 1,1,3,3-tetrakis(dimethylamino)-4-diphenylphosphanyl-1,2-dihydro-3λ5-[1,3]diphosphetium chloride, 2, or, depending on the reaction conditions, the isomer compound 3. The cation of 2 is deprotonated by LiN[Si(CH3)3]2 to give the diphenylphosphanyl-substituted derivative of 1, i.e., compound 4. Methyl iodide adds to 1 to form 1,1,3,3-tetrakis(dimethylamino)-4-methyl-1,2-dihydro-3λ5-[1,3]diphosphetium iodide, 6. Deprotonation of 6 with n-butyllithium leads to the monomethyl derivative of 1, i.e., compound 7. Physical properties, NMR spectra, and mass spectra of compounds 2–4, 6, and 7 are described. The results of the X-ray structural analysis of 6 are reported and discussed. © 1996 John Wiley & Sons, Inc. 相似文献
5.
Reactions of 6-Amino-5-Cyano-3-Methyl-1,4-Diphenyl-1H 4H-Pyrano[2,3-C]Pyrazole and its Methanimidate
Reaction of 6-amino-5-cyano-3-methyl-1,4-diphenyl- 1H,4H-pyrano[2,3-c]pyrazole 1 with triethyl orthoformate in acetic anhydride gave its methanimidate 2, which reacts with primary aliphatic and aromatic amines to give 4,6-dihydro-3-methyl-1,4-diphenyl-6- (alkyl)pyrazolo[4′,3′:5,6]pyrano[2,3-d]pyrimidine-5(lH)- imine 3 and the starting compound 1 , respectively. Treatment of 1 with o-aminophenol gave 5-(2-benzoxalyl)- 1,4-dihydro-3-methyl-1,4-diphenylpyrano[2,3-c]pyrazol- 6-amine 9. 相似文献
6.
Molecular and Crystal Structure of 9λ4-Thia-2,4,6,8,10,11-hexaaza-1λ5,3λ5,5λ5,7λ5-tetraphosphabicylo[5.3.1]undeca-1,3,5,7(11),8,9-hexaene, Cyclotetraphosphazene Bridged by a Sulfur Diimide Group We have carried out an X-ray structure analysis of the title compound ( 1 ). 1 crystallizes in the monoclinic space group P21/b with a = 9.436(4), b = 20.102(7), c = 11.622(5) Å, γ = 103.52(8)°, Z = 8. There are two molecules in the asymmetric unit, which in approximation can be transformed one into the other by additional symmetry elements of a substructure of a space group B2/b. The S = N bond lengths are 1.53 Å. The P? N bonds connecting the SN2 system are 1.666 Å long. They are significantly longer than the P? N multible bonds in the P4N4 ring within a range of 1.517 to 1.565 Å. The sulfur diimide unit and its substituents are coplanar causing a half-boat conformation of the heterocyclic six membered ring. The cyclotetraphosphazene ring shows a flattened crown-saddle conformation, the phosphorous atoms arranged nearly at the corners of a square. Influenced by crystal packing there exist small deviations from the molecular mirror plane and also differences in conformation between the two molecules of the asymmetric unit. 相似文献
7.
1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphete as Ligand in Coordination Compounds 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1 , reacts with GeCl2 · 1,4-dioxane, SnCl2, and (CO)5W(Z-cyclooctene) to give the complexes {HCP[N(CH3)2]2}2 · GeCl2, 3 , {HCP[N(CH3)2]2}2 · SnCl2, 4 , and {HCP[N(CH3)2]2}2 · W(CO)5, 5 , respectively. The n.m.r., mass, and i.r. spectra of the new compounds as well as the crystal and molecular structures of 3 and 4 are reported and the bonding situation in compounds 3–5 is discussed. 相似文献
8.
Diphosphabenzenes. VII. Reactions of 1,1,3,3‐Tetrakis(dimethylamino)‐1 λ5, 3 λ5‐diphosphete with 5‐Cyano‐1‐pentine and 2‐(Cyanomethyl)‐1‐methylpyrrol 5‐Cyano‐1‐pentine reacts with the equimolar amount of the λ5‐diphosphete 1 to give the λ5‐diphosphinine (λ5‐diphosphabenzene) ( 3 ), while reaction with the double equimolar amount of 1 yields the λ5‐diphosphinine ( 4 ). The acyclic compount 6 is the main product of the reaction between 1 and 2‐(cyanomethyl)‐1‐methylpyrrol, 5 . Melting points of 4 · CH3CN and 6 , and mass, nmr and ir spectra of 3 , 4 , and 6 are reported. The crystal structure of 4 · CH3CN shows an open‐chain ylidic CPCP‐sequence, which is linked to a λ5‐diphosphinine via an ethylene bridge. The X‐ray structure analysis of 6 confirms the existence as an acyclic conjugated double ylid. 相似文献
9.
The reaction of sulfene with N,N-disubstituted 3-aminomethylene-2,3-dihydro-4-thiochromanones and-2,3,5,6-tetrahydro-4-thiopyranones gave 1,4-cycloadducts which are derivatives of new heterocyclic systems, namely 3,4-dihydro-5H-[1]benzothiopyrano[3,4-e]-1,2-oxathiin and 3,4,7,8-tetrahydro-5H-thiopyrano[3,4-e]-1,2-oxathiin, respectively. Furthermore, some pyrazole derivatives VII and VIII were prepared from 3-hydroxymethylene-2,3-dihydro-4-thiochromanone or 2,3,5,6-tetrahydro-4-thiopyranone and hydrazines. 相似文献
10.
Ekkehard Fluck Gernot Heckmann Fred Rosche Matthias Westerhausen Ekaterina Gorbunowa 《无机化学与普通化学杂志》1995,621(9):1539-1546
Reactions of λ5-Diphosphetes with COS and CO2. Dihydro-λ5-Phosphetes 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1 , reacts with COS to yield the (3-oxo-3,4-dihydro-1λ5-phosphete-2-yl)-phosphonothioic bis(dimethylamide) 7 . Reaction of dimethyl substituted 1 , i.e. 1,1,3,3-tetrakis(dimethylamino)-2,4-dimethyl-1λ5,3λ5-diphosphete 4 , with COS and CO2 results in (3-oxo-2,3-dihydro-1λ5-phosphete-2-yl)-phosphonothioic bis(dimethylamide) 9 , and (3-oxo-2,3-dihydro-1λ5-phosphete-2-yl)-phosphonic bis(dimethylamide) 10 , respectively. Reaction mechanisms are suggested. 7, 9 and 10 are characterized by their properties, and their nmr, mass-, and ir-spectra. The results of X-ray structural analyses of 9 and 10 are reported and discussed. 相似文献
11.
Palladium(II) Complexes of 1,1,3,3,5,5‐Hexakis(dimethylamino)‐λ5‐[1,3,5]triphosphinine 1,1,3,3,5,5‐Hexakis(dimethylamino)‐1λ5‐3λ5‐5λ5‐[1,3,5]triphosphinine ( 5 ) reacts with (benzonitrile)2PdCl2 to give the chelate complex dichloro(dodeca‐N‐methyl‐1λ5,3λ5,5λ5‐1,3,5‐triphosphinine‐1,1,3,3,5,5‐hexaamin‐C2,C4)palladium ( 6 ). In a pyridine‐d5 solution of 6 the complex dichloro(dodeca‐N‐methyl‐1λ5,3λ5,5λ5‐1,3,5‐triphosphinine‐1,1,3,3,5,5‐hexaamin‐C2)((2H5)pyridine‐N)palladium ( 7 ) is formed. The solute 7 could not be isolated as a solid, because elimination of the solvent regenerates 6 quantitatively. Properties, nmr and ir spectra of 6 and 7 are reported. 6 is characterized by the results of an X‐ray structural analysis. 相似文献
12.
3-Methyl-6,7-dihydro-5H-1,2,4-thiadiazolo[4,5-a]pyrimidine (1) reacted with isoselenocyanates with elimination of acetonitrile and concomitant addition of two molecules of the isoselenocyanate to give 2,3-di-substituted-6,7-dihydro-5H-2aλ4-thia-2,3,4a,7a-tetraazacyclopent[cd]indene-1(2H),4(3H)-diselones (6a)–(6j). 3-Methyl-5,10-dihydrobenzo[e]-1,2,4-thiadiazolo[4,5-a][1,3]diazepine (3) likewise reacted with alkyl isoselenocyanates to give the 2,3-dialkyl-5-10-dihydro-2aλ4-thia-2,3,4a,10a-tetraazapentaleno[3,3a,4-gh]benzocycloheptene-1,4-diselones (9a)–(9h), but reaction of (3) with aryl isoselenocyanates took place with elimination of acetonitrile and incorporation of one molecule of the aryl isoselenocyanate in the product to give 3-arylimino-5,10-dihydro-1,2,4-thiaselenazolo[4,5-b][2,4]benzodiazepines (10a)–(10h). Structure (10) is a new heterocyclic system. The pyrimidine (1) and the diazepine (3) reacted with aryl isoselenocyanates at room temperature in solvents of low polarity to give zwitterion 1:1 addition compounds (7) and (12), respectively. NMR studies reveal that the thiaselenazoles (10) react in solution with aryl isoselenocyanates to give diaryl diselones (11) in a reversible process involving a Dimroth rearrangement. © 1996 John Wiley & Sons, Inc. 相似文献
13.
A. M. Demchenko N. A. Shtil A. P. Andrushko A. N. Krasovsky A. N. Chernega E. B. Rusanov V. V. Pirozhenko M. O. Lozinskii 《Chemistry of Heterocyclic Compounds》2003,39(8):1084-1089
It has been established that the condensation of 3-(4-methoxyphenylamino)-5,6-dihydro-2H-1,4-oxazine with substituted phenacyl bromides occurs at the exocyclic nitrogen atom with formation of 3-aryl-3-hydroxy-1-(4-methoxyphenyl)-2,5,6,8-tetrahydro-3H-imidazo[2,1-c]-1,4-oxazinium bromides. By treatment of the latter with acetic anhydride 3-aryl-1-(4-methoxyphenyl)-5,6-dihydro-8H-imidazo[2,1-c]-1,4-oxazinium bromides are formed. The structures of the compounds synthesized were determined via
1H NMR spectroscopy and X-ray diffraction. 相似文献
14.
Treatment of 5-methylthio-2,3-dihydrothieno[3,2-f]-1,4-thiazepine ( 9 ) with acylhydrazines gave 5,6-dihydrothieno[3,2-f]-1,2,4-triazolo[4,3-d][1,4]thiazepines 10, 11 , and that of 9 with ethyl anthranilate gave 5,6-dihydrothieno[3′,2′:6,7][1,4]thiazepino[5,4-b]quinazolin-8-one ( 14 ). Reaction of 9 with hydrazine hydrate or 4-chlorophenylhydrazine afforded 5-hydrazino compounds 12, 15 , which were subsequently cyclized to ethyl 5,6-dihydrothieno[3,2-f]-1,2,4-triazolo[4,3-d][1,4]thiazepine-3-carboxylate ( 13 ), 2-(4-chlorophenyl)-5,6-dihydrothieno[3,2-f]-1,2,4-triazolo[4,3-d][1,4]thiazepin-3(2H)-one ( 16 ) and 2-(4-chlorophenyl)-6,7-dihydro-2H-thieno[3,2-f][1,2,4]triazino[4,3-d][1,4]thiazepine-3,4-dione ( 17 ). New thieno-anellated heterocycles were prepared with the aim of studying their affinity for the benzodiazepine receptors. 相似文献
15.
Z. G. Aliev A. N. Maslivets O. P. Krasnykh Yu. S. Andreichikov L. O. Atovmyan 《Russian Chemical Bulletin》1993,42(9):1569-1572
Thermal decarboxylation of 3-p-toluoyl-1,2-dihydro-4H-pyrrolo[5,1-c][1,4]benzoxazine-1, 2,4-trione resulted in 2-oxo-2H-1,4-benzoxazin-3-yl(p-toluoyl)ketene; the latter under-goes [4+2]-cycloaddition withp-bromobenzaldehyde to form 1-p-bromophenyl-4-p-toluoyl-1, 3-dihydro-5H-[1,3]oxazino[4,3-c][1,4] benzoxazine-3,5-dione. The crystal and molecular structure of the latter has been studied by X-ray analysis.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1633–1636, September, 1993. 相似文献
16.
The dipolar 1,4-cycloaddition of dichloroketerie to N,N-disubslituled 3-aminomethylene-2,3-dihydro-4-thiochromanones and 3-aminomethylenetelrahydro-4-thiopyranones gave N,N-disubstituted 4-amino-3,3-diehloro-3,4-dihydro-2H,5H-[1]benzolhiopyrano[4,3-b]pyran-2-ones and 4-amino-3,3-dichloro-3,4,7,8-tetrahydro-2H,5H-thiopyrano[4,3-b]pyran-2-ones, respectively, only in the ease of aromatic or strong hindering aliphatic N-substitution. The adducts gave N,N′-disubstituted 4-amino-3-chloro-2H,5H-[1]benzothiopyrano[4,3-b]pyran-2-ones and 4-amino-3-chloro-7,8-dihydro-2H,5H-thiopyrano[4,3-b]pyran-2-ones, respectively, by dehydro-chlorination with DBN. By chromatography on neutral alumina, 3-(2,2-dichloroethylidene)-2,3-dihydro-4-thiochromanone was isolated as an unstable liquid from the reaction between dichloroketerie and 3-diethylaminornethylene-2,3-dihydro-4-thiochromanone. 相似文献
17.
Avelina Ong-Lee Leo Sylvester Jan W. F. Wasley 《Journal of heterocyclic chemistry》1983,20(6):1565-1569
1,3,4,14b-Tetrahydro-2H,10H-pyrazino[1,2-α]pyrrolo[2,1-c] [1,4]benzodiazepines (1a-e) were synthesized to investigate their potential CNS activity. The key step in the synthesis was the formation of the 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine (13) by reduction and concomitant cyclization of the nitroketone (11). Biological evaluation of 1a-e revealed interesting properties for 1b (CGS 7525A) [2]. 相似文献
18.
Christophe Chdru Bernard Decroix Jean Morel Frantisek Povazanec 《Journal of heterocyclic chemistry》1994,31(4):1027-1032
The 5,10-dihydro-4H-furo[3,2-e]pyrrolo[1,2-α][1,4]diazepin-5-one ( 7 ) and furo[3,2-e]pyrrolo[1,2-α][1,4]diaze-pine ( 10 ) are synthesized from suitable isocyanates 3a,b in acetic acid. The reactivity of 10 (C- and N-alkyla-tion) is investigated. 相似文献
19.
Piergiorgio Pecorari Marcella Rinaldi M. Paola Costi Luciano Antolini 《Journal of heterocyclic chemistry》1992,29(6):1449-1455
Derivatives of two new molecular structures, namely, 7,8-dihydro-6H,10H-[1,2,5]thiadiazolo[3′,4′:4,5]pyrimido[2,1-b][1,3]thiazin-10-one and 6,7-dihydro-9H-thiazolo[3,2-a][1,2,5]thiadiazolo[3,4-d][pyrimidin-9-one, and derivatives of N-substituted sulfamic acid, namely, (8-amino-3,4-dihydro-2H,6H-pyrimido[2,1-b][1,3]thiazin-6-on-7-yl)sulfamic acid and (7-amino-2,3-dihydro-5H-thiazolo[3,2-a]pyrimidin-5-on-6-yl)sulfamic acid, were separated out as by-products in the reduction reaction of 8-amino-3,4-dihydro-7-nitroso-2H,6H-pyrimido[2,1- b][1,3]thiazin-6-one and 7-amino-2,3-dihydro-6-nitroso-5H-thiazolo[3,2-a]pyrimidin-5-one derivatives, respectively, with sodium hydrosulfite. A mechanism of reaction, which hypothesizes the action of sodium hydrosulfite in an asymmetic form, is proposed. The results of single-crystal X-ray investigation on 7,8-dihydro-6H,10H-[1,2,5]thiadiazolo[3′,4′:4,5]pyrimido[2,1-b][1,3]thiazin-10-one (R = 0.032 for 863 reflections) and (8-amino-3,4-dihydro-2H,6H-pyrimido[2,1-b]- [1,3]thiazin-6-on-7-yl)sulfamic acid, sodium salt (R = 0.028 for 3507 reflections) are reported. 相似文献
20.
Istvn Hermecz Ildik Szilgyi Lszl Orfi Jzsef Kksi Gyrgy Szsz 《Journal of heterocyclic chemistry》1993,30(5):1413-1420
3,4-Dihydro-1H,6H-[1,4]oxazino[3,4-b]quinazolin-6-one 3 and its 1-methyl and 1-hydroxy derivatives 8 and 13 were prepared by different routes. The active methylene group of compound 3 was reacted with electro-hilic reagents (bromine, phenyldiazonium chloride, nitrous acid, a Vielsmeier-Haack reagent, aromatic aldehydes and diethyl oxalate) to yield 1-substituted-3,4-dihydro[1H,6H)-1,4-oxazino[3,4-b]quinazo-lin-6-ones. The reactivity of 1-hydroxy and 1-bromo derivatives 13 and 15 were also investigated in some reactions. The 3,4-dihydro-lH,6H-[1,4]oxazino[3,4-b]quinazolin-6-ones were characterized by means of uv, 1H and 13C nmr spectroscopy. 相似文献