4-Substituted-4H-pyrrolo[2,1-c] [1,4]benzoxazines

The condensations of 1-(2-hydroxyphenyl) pyrroles with a variety of carbonyl compounds are shown to give new 4-substituted-4H-4-methylpyrrolo[2,1-c][1,4]benzoxazines. Some of the products were further functionalized. The ir, uv, and pmr spectra of the title heterocyclic system are discussed. Reaction of 1-(2-hydroxyphenyl) pyrrole with dimethyl acetylenedicarboxylate yielded dimethyl 3-(2-hydroxyanilino) phthalale; a mechanistic rationale which accounts for the result involves a rearrangement of the hypothetical Diels-Alder adduct.     

Zur Kenntnis der Na5[GaO4]-Verwandtschaft: KNa4[GaO4] und CsK4[GaO4]

About the Na₅[GaO₄]-Relationship: KNa₄[GaO₄] and CsK₄[GaO₄] KNa₄[GaO₄] was newly prepared from binary oxides (powders) and also from KGaO₂/Na₂O/K₂O (colourless columnar single crystals) in a closed Ag-cylinder at 600 and 650°C. Space group Pbca with a = 1046.1(2), b = 596.3(1), c = 1871.1(3) pm, Z = 8 [Four-circle-diffractometer data, 1138 I₀(hkl), MoKα, R = 8.29, R_w = 6.76%, anisotropic refinement] (Parameter s. text). Colourless cubic single crystals of hitherto unknown CsK₄[GaO₄] are formed by reaction of K₂O, CsGaO₂, and Cs₂O (surplus) in a closed Au-tube at 580°C. Space group Pbca with a = 1154.7, b = 667.7, c = 2096.6 pm, Z = 8 [Four-circle-diffractometer data, 1798 I₀(hkl), MoKα, R = 7.62, R_w = 7.68%, anisotropic refinement] (Parameter s. text). Both crystal structures belong to the Na₅[GaO₄] type. Structural aspects, ECoN, and MAPLE of KNa₄[GaO₄] and CsK₄[GaO₄] in relation with Na₅[GaO₄] are discussed.     

Properties of 4H-[1]benzopyrano[3,4-c]-[1,2,5]-selenodiazol-4-one

4H-[1]benzopyrano[3,4-c][1,2,5]selenodiazol-4-one has been synthesized by the reaction of 3,4-diaminocoumarin with selenous acid and its reaction with several nucleophiles (alkali, ammonia, amines, hydrazine hydrate) and its nitration have been studied. Using PMR spectroscopy, a comparative kinetic study of the opening of the lactone ring in 6,8-dinitro-4H-[1]benzopyrano[3,4-c][1,2,5]seleno- and thiadiazol-4-ones has been carried out.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 128–133, January, 1991.     

Porphyrin-Calix[4]arenes

The review deals with the synthesis, chemical modification, and complexing properties of a new class of molecular receptors, porphyrin-calix[4]arene conjugates.__________Translated from Zhurnal Organicheskoi Khimii, Vol. 41, No. 6, 2005, pp. 807–826.Original Russian Text Copyright © 2005 by Mamardashvili, Koifman.     

Calix[4]azulene

Azulene reacts with paraformaldehyde in the presence of florisil to give excellent yields of calix[4]azulene.     

Structural features of Ag[AuF4] and Ag[AuF6] and the stuctural relationship of Ag[AgF4]2 and Au[AuF4]2 to Ag[AuF4]2

Synchrotron radiation X-ray powder diffraction data (SPDD) have been obtained for Ag[AgF4]2, Au[AuF4]2, Ag[AuF4], and Ag[AuF6]. Ag[AgF4]2 and Au[AuF4]2 are isostructural with Ag[AuF4]2, space group (SG) P2(1)/n, Z = 2, with the following: for Ag[AgF4]2 a = 5.04664(8), b = 11.0542(2), c = 5.44914(9) A, beta = 97.170(2) degrees; for Au[AuF4]2 a = 5.203(2), b = 11.186(3), c = 5.531(2) A, beta = 90.55(2) degrees. The structure of Ag[AgF4]2 was refined successfully (SPDD) applying the Rietveld method, yielding the following interatomic distances (A): AgII-F = 2.056(12), 2.200(13), 2.558(13); AgIII-F = two at 1.846(12), others = 1.887(12), 1.909(13), 2.786-(12), 2.796(12), 2.855(12). AgAuF4, like other AA'F4 salts (A = Na-Rb; A' = Ag, Au), crystallizes in the KBrF4 structure type, SG I4/mcm (140), Z = 4 with a = 5.79109(6), c = 10.81676(7) A. SPDD gave (in A) four AuIII-F = 1.89(1) and eight AgI-F = 2.577(7). SPDD for AgAuF6 confirmed that it has the LiSbF6 structure, SG R3, Z = 3, with a = 5.2840(2), c = 15.0451(6) A.     

Das erste Oxid vom Formeltyp K5[MO4]: K5[TIO4] [1]

The First Oxide with the Formula Type K₅[MO₄]: K₅[TlO₄] Light yellow powder and pale yellow transparent single crystals of K₅[TlO₄] were newly prepared from mixtures of binary oxides (K₂O/Tl₂O₃) preheated and levigated several times [closed Ag-cylinder, 580°C, 24 h and 600°C, 20 d]. Space group Pbca with a = 1170.4(3), b = 686.1(1), c = 2079.2(5) pm, Z = 8 [four-circle-diffraktometer data, 997 I₀(hkl), R = 7.87%, R_w = 5.63%, MoKα] (parameter s. text). The crystal structure belongs to the Na₅[GaO₄] type. Structural aspects, ECoN and MAPLE are discussed.     

Microwave-assisted synthesis of resorcin[4]arene and pyrogallol[4]arene macrocycles

A series of resorcin[4]arene and pyrogallol[4]arene macrocycles have been synthesized efficiently within 5 min, affording crystalline products suitable for single crystal X-ray diffraction, utilising microwave irradiation in a ‘one-pot’ reaction whilst controlling the selective formation of the rccc cone stereoisomer.     

Synthesis and self-assembly of novel calix[4]arenocrowns: formation of calix[4]areno[2]catenanes

A series of novel calix[4]arenocrowns 1a-c were efficiently synthesized by a one-pot reaction of calix[4]monohydroquinone diacetate 5 with ditosylate 6 and its analogues in the presence of sodium hydroxide. It was found that the calix[4]arenocrowns could form stable pseudorotaxane-type complexes 2a-c with paraquat, and further self-assemble into calix[4]areno[2]catenanes 3a-c with dicationic salt 8 and p-bis(bromomethyl)benzene.     

Fourfold [2]rotaxanes based on calix[4]arenes

Tetraurea calix[4]arenes with four loops form exclusively heterodimers with open-chain urea calix[4]arenes when they are dissolved in aprotic solvents. These assemblies can be considered as pseudorotaxanes. If open-chain tetraureas ending with maleic imide functions are used, their Diels-Alder reaction with 1,4,5,8-tetrapentoxyanthracene leads to tetra[2]rotaxanes which cannot be split into the single calixarene parts by hydrogen bond breaking solvents.