共查询到20条相似文献,搜索用时 31 毫秒
1.
M. Botta M. Cavalieri D. Ceci F. De Angelis G. Finizia R. Nicoletti 《Tetrahedron》1984,40(17):3313-3320
The synthesis of 6-alkyl and 5,6-dialkyl-2-methoxy-4(3H)-pyrimidinones 3 is described. Their versatility to be transformed into 6-alkyl and 5,6-dialkyluracils 4(a-h), 6-alkyl and 5,6-dialkyl-3-methyluracils 7(a,e,f) and 6-alkyl and 5,6-dialkyl-2-alkoxy-4(3H)-pyrimidinones 5(a-i) is also shown. 相似文献
2.
Methyl (E)-4,4-dimethyl-5-oxo-2-pentenoate ( 1 , X = O) reacted with 1,2- or 1,3-aminoalcohols 3 to yield oxazolidines 4a-c or tetrahydro-1,3-oxazines 4d,e. The corresponding imino ester 1 (X = NBu-t) also gave 4 on reaction with 3 . Compounds 4 on heating at 230° yielded 4,5-dihydrooxazoles 5a-c or 5,6-dihydro-4H-1,3-oxazines 5d,e along with methyl 4-methyl-3-pentenoate ( 6 ). 相似文献
3.
Yoichi Yamada Heinosuke Yasuda Yuichi Yoshihara Kazue Yoshizawa 《Journal of heterocyclic chemistry》1999,36(5):1317-1321
A series of ethyl 7-amino-2,4-dioxopteridine-6-carboxylates 4 and ethyl 7-amino-4-oxo-2-thioxopteridine-6-carboxylates 5 , of interest biologically, has been prepared in one step from the reaction of such vicinal-diamines as 1,3-dialkyl-5,6-diaminouracils 2 or 1,3-dialkyl-5,6-diamino-2-thiouracils 3 with diethyl (E)-2,3-dicyanobutenedioate ( 1 ). Moreover, ethyl 3-amino[1,2,4]triazino[2,3-a]-1H-benzimidazole-2-carboxylate ( 11 ) was also obtained from the reaction between 1,2-diamino-1H-benzimidazole ( 10 ) and 1 . The structural studies of 4, 5 , and 11 prepared were carried out by nmr experiments in some details. 相似文献
4.
L. A. Ignatova A. E. Gekhman P. L. Ovechkin B. V. Unkovskii 《Chemistry of Heterocyclic Compounds》1974,10(3):307-309
3,4,4,6-Tetramethyl-2-aryliminotetrahydro-1,3-oxazines were synthesized by intramolecular cyclization of N-aryl-N′-methyl-N′-(2-methyl-4-hydroxy-2-pentyl)-S-methylisothioureas. 4,4,6-Trimethyl-2-(N-methyl-N-arylamino)-5,6-dihydro-4H-1,3-oxazines were obtained by methylation of 4,4,6-trimethyl-2-arylamino-5,6-dihydro-4H-1,3-oxazines. 相似文献
5.
The transition-metal-carbonyl-induced cyclodimerization of 5,6-dimethylidene-7-oxabicyclo[2.2.1]hept-2-ene is strongly affected by substitution at C(1) While 5,6-dimethylidene-7-oxabicyclo[2.2.1]hept–2-ene-l-methanol ( 7 ) refused to undergo [4 + 2]-cyclodimerization in the presence of [Fe2(CO)9] in MeOH, 1-(dimethoxymethyl)-5,6-di-methylidene-7-oxabicyclo[2.2.1]hept-2-ene ( 8 ) led to the formation of a 1.7:1 mixture of ‘trans’ ( 19, 21, 22 ) vs. ‘cis’ ( 20, 23, 24 ) products of cyclodimerization together with tricarbonyl[C, 5,6, C-η-(l-(dimethoxymethyl)-5,6-di-methylidenecyclohexa-1,3-diene)]iron ( 25 ) and tricarbonyl[C,3,4, C-η-(methyl 5-(dimethoxymethyl)-3,4-di-methylidenecyclohexa-1,5-diene-l-carboxylate)]iron ( 26 ). The structures of products 19 and of its exo ( 21 ) and endo ( 22 ) [Fe(CO)3(1,3-diene)]complexes) and 20 (and of its exo ( 23 ) and endo (24) (Fe(CO)3(1,3-diene)complexes) were confirmed by X-ray diffraction studies of crystalline (1RS, 2SR, 3RS, 4RS, 4aRS, 9aSR)-tricarbonyl[C, 2,3, C-η-(1,4-epoxy-1,5-bis(dimethoxymethyl])-2,3-dimethylidene-1,2,3,4,4a,9,9a,10-octahydroanthracene)iron ( 21 ). In the latter, the Fe(CO)3(1,3-diene) moiety deviates significantly from the usual local Cs symmetry. Complex 21 corresponds to a ‘frozen equilibrium’ of rotamers with η-alkyl, η3-allyl bonding mode due to the acetal unit at the bridgehead centre C(1). 相似文献
6.
Kaylene M. Pritchard 《合成通讯》2013,43(23):4076-4096
We now report the first reaction of Ph3P(SCN)2 with 4,6-dihydroxy-5-methylisophthalic acid to give 10-methyl-2,8-dithio-1,3-oxazino-1,3-benzoxazine-4,6-dione. Also, the enol tautomer has been utilized in the reaction of β-keto acids with Ph3P(SCN)2 to give novel 2-thio-1,3-oxazines. Subsequent reaction of the 2-thio-1,3-oxazines with benzylamine resulted in opening of the oxazine ring and gave novel dibenzylamino-enamides, which could be cyclized to thiouracils. The reaction of 2-thio-1,3-oxazines with morpholine at low temperature led to the production of unstable 2-Mercapto-2-morpholino-1,3-oxazines. 2-Mercapto-2-morpholin-4-yl-2,3,5,6,7,8-hexahydro-4H-1,3-benzoxazin-4-one was observed to lose H2S at room temperature to give 2-morpholin-4-yl-5,6,7,8-tetrahydro-4H-1,3-benzoxazin-4-one, which was subsequently tested and found to exhibit some antiplatelet activity. 相似文献
7.
The configurations and conformations of cis- and trans-N-methyl- and -N-benzyl-4,5- and -5,6-tetramethylenetetrahydro-1,3-oxazines were determined by 1H and 13C NMR spectroscopy. The cis isomers are conformationally homogeneous, having the hetero atom attached to the cyclohexyl ring, in the axial and equatorial positions, respectively, in the 5,6- and 4,5-tetramethylene compounds, similar to the case of the 2-p-nitrophenyl-substituted analogues investigated previously. 相似文献
8.
Beyhan Yiğit Murat Yiğit İsmail Özdemir Engin Çetinkaya 《Transition Metal Chemistry》2012,37(3):297-302
Three RuCl2(η6-arene, η1-carbene) and two RuCl2(NHC)(arene) complexes have been prepared by the reaction of bis(1,3-dialkylperhydrobenzimidazol-2-ylidene) (1) and bis(1,3-dialkyl-4-methylzimidazolin-2-ylidene) (3) with [RuCl2(arene)]2 in toluene and characterized by elemental analysis, 1H NMR, 13C NMR and IR spectroscopy. The catalytic activities of these complexes were examined in the transfer hydrogenation of aromatic
ketones using 2-propanol as hydrogen source. 相似文献
9.
About Chemistry and Structure of Olefin-monocyano-dicarbonyl-ferrate Anions By the reactions of olenFe(CO)3 [olen = C5H8(isoprene), C7H10(cycloheptadiene-1,3), C8H14(2,5-dimethylhexadiene-1,3)] with sodium bis [trimethylsilyl]amide the new anions [olenFe(CO)2CN]? are formed. All so far known [olenFe(CO)2CN]? complexes [olen = C5H8(isoprene), C7H10[cycloheptadiene-1,3], C4H6(butadiene), C5H8(pentadiene-1,3), C6H8(cyclohexadine-1,3), C6H10(2,3-dimethylbutadiene), C8H8(cyclooctatetraene)] have fluctional structures in solution as shown by 13C NMR spectroscopic investigations. At low temperatures only the isomer exists, in which the CN? ligand and one of the two CO molecules occuppy the basal positions of a square pyramide together with 2 C atoms of the diene part. 相似文献
10.
S. V. Gorbunov T. O. Denisova E. V. Amel’chenkova S. E. Nefedov 《Russian Journal of Inorganic Chemistry》2006,51(10):1581-1586
We found that the reaction of the compound obtained by alloying hydrous cobalt(II) acetate and pivalic acid with 3-methyl-5-pyrazolone in refluxing hexane produces the tetranuclear complex Co4(μ3-OH)2(μ-OOCBut)6·(C4H6N2O)4·2HOOCBut (complex 3). The complex has been structurally characterized using single-crystal X-ray diffraction 相似文献
11.
Masood Parvez Veejendra K. Yadav Govindaraji Senthil 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(1):82-85
6-Vinyl-1-oxa-4-thiaspiro[4.5]dec-6-ene has been reacted with dienophiles, such as N-phenylmaleimide (NPM), N-methyltriazoline-2,5-dione (MTAD) and dimethylacetylene dicarboxylate (DMAD), to assess the 1,3-diastereofacial selection caused by the acetal function. In each case, a mixture of two diastereoisomers was produced. The crystal structures of the products of the addition of NPM and MTAD syn to the acetal oxygen, 2-phenyl-2,3,3a,4,5,5a,6,7,8,9,9a,9b-dodecahydro-1H-benz[e]isoindole-6-spiro-2′-[1′,3′]oxathiolane-1,3-dione, C20H21NO3S, (IIa), and 2-methyl-5,7,8,9,10,10a-hexahydro-1H-1,2,4-triazolo[1,2-a]cinnoline-7-spiro-2′-[1′,3′]oxathiolane-1,3-dione, C13H17N3O3S, (IIIa), respectively, and the product of the addition of DMAD syn to the acetal sulfur, dimethyl 1,2,3,4,4a,7-hexahydronaphthalene-1-spiro-2′-[1′,3′]oxathiolane-5,6-dicarboxylate, C16H20O5S, (IVb), have been determined. All three structures are composed of independent molecules separated by normal van der Waals distances. The 1-oxa-4-thia heterocyclic ring has an envelope conformation in the three structures and the S—Csp3 bond distances differ significantly from each other, as observed in comparable structures; the remaining molecular dimensions are as expected. 相似文献
12.
Murat Yiğit Ismail Özdemir Engin Çetinkaya Bekir Çetinkaya 《Transition Metal Chemistry》2007,32(4):536-540
Reaction of 1,3-dialkylperhydrobenzimidazolinylidene, 1,3-dialkyl-4-methylimidazolinylidene and 1,3-dialkylimidazolinylidene
with [RhCl(COD)]2 yields {1,3-dialkylperhydrobenzimidazolin-2-ylidene}-, {1,3-dialkyl-4-methylimidazolin-2-ylidene}- {1,3-dialkylimidazolin-2-ylidene}chloro(η4-1,5-cyclooctadiene)rhodium(I) complexes (2a–c) and (4a, b). All compounds synthesised were characterised by elemental analysis, n.m.r. spectroscopy. Phenylboronic acid reacts with
aldehydes in the presence of a catalytic amount of the new rhodium(I)–carbene complexes (2a–c) and (4a, b), to give the corresponding aryl secondary alcohols in good yield (73–99%). 相似文献
13.
IR-spectroscopic measurements between ?60° and 0°C show the existence of C6H5J(OAc)2-n(N3)n generated by the reaction of C6H5J(OAc)2 with (CH3)3SiN3. C6H5J(OAc)2-n(N3)n reacts with 2,3-dimethylbutad to give substances C12H20N6 (1), having the probable structure of 2,3,5-trimethyl-3,6-di-azidomethyl-heptadiene-1,5 and 3,4-diazido-3-methylbutanone-2 (2). Likewise we get from 1,3-cyclohexadiene the diazide C12H16N6 (3), and 4-azido-cyclohexene-2-on-1 (4). Analogously from cyclopentadiene we get the carbonylcompound 4-azido-cyclopentene-2-on-1 (5). E-5-azido-hexene-3-on (8) results from 2,4-E,Z-hexadiene. 1,3-cyclooctadiene gives as main product 6 (4-azido-cyclooctene-2-on-1) but also some 7 (8-azido-cyclooctene-2-on-1) emerging from an attack on positions 1 and 2.Δ1,3, Δ3,5 and Δ4,6-cholestadiene yield in a regio- and stereo-specific manner the products 9 (1α-azidocholestene-2-on-4), 10 (6β-azidocholestene-4-on-3) and 11 (4β-azidocholestene-5-on-7). These last examples confirm our suggestions from the preponderance of the 1,4-functionalisation. 相似文献
14.
《Tetrahedron》1987,43(12):2709-2720
The electrochemical reduction of 2-phenyl-6H-1,3-thiazines carried out at a mercury cathode in acetate buffer + ethanol (1:1) has been studied : - In the case of compounds monoactivated at carbon 5 (R5 = CHO or COCH3) either hydrodimers (resulting from coupling at C-2), 3,6-dihydro-2H-1,3-thiazines (reduction of the imine bond) or tetrahydrothiazines can be obtained. - Diactivated 6H-1,3- thiazines (R4 = CO2Et, R5 = CHO or COCH3) successively lead to 5,6-dihydro-4H-1,3-thiazines (reduction of the ethylenic bond) and tetrahydrothiazines. - The reduction of a 6H-1,3-thiazine bearing only one withdrawing group at carbon 4 gives rise to a ring opening. At the same time, the action of various chemical reducing agents has been examined : the reduction of the imine bond is performed using NaBH3CN while NaBH4 or LiAlH4 leads to the reduction of the substituents on the heterocyole. 相似文献
15.
Nenad S. Draškovi Miloš I. Djuran Milica S. Cvijović Dušanka D. Radanović Violeta Jevtović 《Transition Metal Chemistry》2004,29(8):874-879
Starting from Ba2(1,3-pddadp)·8H2O (1,3-pddadp=1,3-propanediamine-N,N′-diacetate-N,N′-di-3-propionate ion) and CoSO4, a new hexadentate [CoII(1,3-pddadp)]2− complex has been prepared. The trans(O6) geometry of this complex was confirmed by comparison of its i.r. and u.v.–vis. spectra with those of [CoII(1,3-pdta)]2− (1,3-pdta is the 1,3-propanediaminetetraacetate ion) and trans(O6)-[CoIII(1,3-pddadp)]− complexes of known X-ray crystal structure. Magnetic and electrolytic conductivity properties of these complexes have also been discussed. 相似文献
16.
Rafal Kruszynski Agata Trzesowska‐Kruszynska 《Acta Crystallographica. Section C, Structural Chemistry》2009,65(12):o624-o629
The 2‐aminobenzothiazole sulfonation intermediate 2,3‐dihydro‐1,3‐benzothiazol‐2‐iminium monohydrogen sulfate, C7H7N2S+·HSO4−, (I), and the final product 2‐iminio‐2,3‐dihydro‐1,3‐benzothiazole‐6‐sulfonate, C7H6N2O3S2, (II), both have the endocyclic N atom protonated; compound (I) exists as an ion pair and (II) forms a zwitterion. Intermolecular N—H...O and O—H...O hydrogen bonds are seen in both structures, with bonding energy (calculated on the basis of density functional theory) ranging from 1.06 to 14.15 kcal mol−1. Hydrogen bonding in (I) and (II) creates DDDD and C(8)C(9)C(9) first‐level graph sets, respectively. Face‐to‐face stacking interactions are observed in both (I) and (II), but they are extremely weak. 相似文献
17.
Min Min Zhao Zhi Rong Qu 《Acta Crystallographica. Section C, Structural Chemistry》2010,66(7):m188-m190
The reaction of propane‐1,3‐diamine hydrochloride, 18‐crown‐6 and zinc(II) chloride in methanol solution yields the title complex salt [systematic name: propane‐1,3‐diaminium tetrachloridozincate(II)–1,4,7,10,13,16‐hexaoxacyclooctadecane (1/1)], (C3H12N2)[ZnCl4]·C12H24O6, with an unusual supramolecular structure. The diprotonated propane‐1,3‐diaminium cation forms an unexpected 1:1 supramolecular rotator–stator complex with the crown ether, viz. [C3H12N2(18‐crown‐6)]2+, in which one of the –NH3+ substituents nests in the crown and interacts through N—H...O hydrogen bonding. The other –NH3+ group interacts with the [ZnCl4]2− anion via N—H...Cl hydrogen bonding, forming cation–crown–anion ribbons parallel to [010]. 相似文献
18.
The loss of CH3˙ from the molecular ions of cyclohexene oxide and 5,6-dihydro-4-methyl-2H-pyran has been investigated. On the basis of metastable peak shape analysis, collision-induced dissociation/mass-analysed ion kinetic energy spectra and thermochemical data it is concluded that the same [C5H7O]+ ion is formed in both cases. 相似文献
19.
Masataka Yokoyama Hiroshi Inazawa Tomoji Shimizu Masahito Kodera Tsuneo Imamoto 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-2):187-193
Abstract Two 1,3-oxazine-6-thione derivatives obtained by “S,N-Double Rearrangement2” reacted with several nucleophiles to produce 1,3-diazin-6-ones, 6-imino-1,3-oxazines, 1,3,4-triazoles, 1,2,4-oxadiazoles, and 1,3-thiazol-6-ones. Their ring transformations are discussed. 相似文献
20.
V. M. Kisel' V. A. Kovtunenko L. M. Potikha A. V. Turov 《Chemistry of Heterocyclic Compounds》1995,31(4):457-460
It has been shown that nucleophilic reagents react with the 6-methyl-5-oxoisoquino[2,3-a]quinazolinium cation at the C(2) atom. The structure of the reaction product is determined by the type of reagent. On reaction with sodium borohydride and secondary amines, 12H- and 12-dialkylamino-12H-6-methyl-5-oxo-5, 6-dihydroisoquino[2,3-a]quinazolines are formed. In the case of primary amines the reaction is accompanied by fission of the C(12)-N(t3) bond with the formation of 2-[o-(N-alkylformimidoyl)-benzyl]-3-methyl-4-oxoquinazolines.See [1) for the preceding communication.T. G. Shevchenko Kiev University, Kiev 252017. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 522–526, April, 1995. Original article submitted March 24, 1995. 相似文献