scholarly journals Synthesis and characterization of 3-methyl-6-[(propynyloxy)methyl]-1,4-dioxane-2,5-dione

2017 ◽  
Vol 73 (7) ◽  
pp. 1044-1047
Author(s):  
Igor Elkin ◽  
Thierry Maris ◽  
Patrice Hildgen
Keyword(s):  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Dimensional Structure ◽  
Axial Position ◽  
Synthesis And Characterization ◽  
Boat Conformation ◽  
Dione Derivative ◽  
Derivatives Of ◽  
Twist Boat

The number of known asymmetrically substituted hemilactides, important precursors for obtaining regular derivatives of polylactide polymers, is still limited and structural characterization of most of them is incomplete. In the title racemic 1,4-dioxane-2,5-dione derivative, C9H10O5, the hemilactide heterocycle exhibits a twist-boat conformation. The bulkier propynyloxymethyl group is in an axial position with agaucheconformation for the CH2–O–CH2–C segment. In the crystal, molecules are linked by pairs of C—H...O hydrogen bonds, forming inversion dimers. The dimers are linked by further C—H...O contacts, forming a three-dimensional structure.

scholarly journals 3-Hydroxy-4-phenyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one:cisisomer

IUCrData ◽  
2016 ◽  
Vol 1 (11) ◽  
Author(s):  
Mohammed Rida ◽  
Youness El Bakri ◽  
Mohamadou Lamine Doumbia ◽  
Mohammed Benchidmi ◽  
El Mokhtar Essassi ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Title Compound ◽  
Three Dimensional ◽  
Dimensional Structure ◽  
Boat Conformation ◽  
Aromatic Rings ◽  
Three Dimensional Structure ◽  
Π Interactions ◽  
Compound C ◽  
Twist Boat

In the title compound, C15H14N2O2, the seven-membered benzodiazepine ring adopts a twist-boat conformation and the two aromatic rings are inclined to one another by 81.06 (15)°. In the crystal, molecules are linked by N—H...O hydrogen bonds, forming chains propagating along the [10-1] direction. The chains are linked by C—H...O hydrogen bonds, forming sheets parallel to theacplane. Within the sheets, there are N—H...π interactions present, and C—H...π interactions link the sheets to form a three-dimensional structure.

A concise and efficient concurrent synthesis of 6,11-dihydrodibenzo[b,e]azepines and 5,6,11,12-tetrahydrodibenzo[b,f]azocines and their conversion to 4-oxo-8,13-dihydro-4H-benzo[5,6]azepino[3,2,1-ij]quinoline-5-carboxylates and N-acetyl-5,6,11,12-tetrahydrodibenzo[b,f]azocines: synthetic sequence, spectroscopic characterization and the structures of two products

2019 ◽  
Vol 75 (6) ◽  
pp. 650-656
Author(s):  
Lina M. Acosta Quintero ◽  
Alirio Palma ◽  
Justo Cobo ◽  
Christopher Glidewell
Keyword(s):  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Spectroscopic Characterization ◽  
Boat Conformation ◽  
Framework Structure ◽  
Molar Ratios ◽  
Boat Form ◽  
Synthetic Sequence ◽  
Time Form ◽  
Twist Boat

Reaction of 2-allyl-N-benzyl-4-fluoroaniline or 2-allyl-N-benzyl-4-chloroaniline with 98% sulfuric acid leads to the concurrent formation of halogeno-substituted 11-ethyl-6,11-dihydrodibenzo[b,e]azepines, (II), and halogeno-substituted 11-methyl-5,6,11,12-tetrahydrodibenzo[b,f]azocines, (III), in each case in (II):(III) molar ratios of ca 2:1. Further reaction of (II) leads to ethyl 13-ethyl-2-halogeno-4-oxo-8,13-dihydro-4H-benzo[5,6]azepino[3,2,1-ij]quinoline-5-carboxylate, while acetylation of (III) gives the corresponding N-acetyl derivatives. The dibenzo[b,e]azepine and dibenzo[b,f]azocine ring systems are of importance in forming the core of a variety of bioactive compounds. In ethyl 13-ethyl-2-fluoro-4-oxo-8,13-dihydro-4H-benzo[5,6]azepino[3,2,1-ij]quinoline-5-carboxylate, C22H20FNO3, (IVa), the azepine ring adopts a conformation close to the twist-boat form, and the molecules are linked into a three-dimensional framework structure by a combination of C—H...O and C—H...π(arene) hydrogen bonds. The azocine ring in 5-acetyl-2-chloro-11-methyl-5,6,11,12-tetrahydrobenzo[b,f]azocine, C18H18ClNO, (Vb), adopts the boat–boat conformation and the molecules are again linked by C—H...O and C—H...π(arene) hydrogen bonds, but this time form a sheet structure.

scholarly journals Synthesis and crystallographic characterization of a mononuclear cobalt(III) complex possessing both thiolate and thioether donors: reactivity of an thiolate-bridged pentanuclear Co2Ag3complex with iodomethane

2017 ◽  
Vol 73 (5) ◽  
pp. 678-681
Author(s):  
Yosuke Fukuda ◽  
Nobuto Yoshinari ◽  
Takumi Konno
Keyword(s):  
Hydrogen Bonds ◽  
Title Compound ◽  
Three Dimensional ◽  
Mononuclear Complex ◽  
The Other ◽  
Dimensional Structure ◽  
Cationic Complex ◽  
Three Dimensional Structure ◽  
Mononuclear Cobalt

Treatment of an S-bridged pentanuclear AgI3CoIII2complex, [Ag3{Co(L)}2]3+[L3–= N(CH2NHCH2CH2S−)3], in which two tris(thiolate)-type mononuclear CoIIIunits ([Co(L)]) are bridged by three AgIions through S atoms, with iodomethane (CH3I) gave a new CoIIImononuclear complex, [Co(LMe2)]2+[LMe2−= N(CH2NHCH2CH2S−)(CH2NHCH2CH2SCH3)2], systematic name: {2-[(bis{[2-(methylsulfanyl)ethyl]aminomethyl}aminomethyl)amino]ethanethiolato}cobalt(III) bis(hexafluoridophosphate). This cationic complex was crystallized with PF6−anions to form the title compound, [Co(LMe2)](PF6)2. In the [Co(LMe2)]2+cation, two of three thiolate groups in [Co(L)] are methylated while one thiolate group remains unreacted. Although a total of eight stereoisomers are possible for [Co(LMe2)]2+, only a pair of enantiomers {ΛRR- and ΔSS-[Co(LMe2)]2+} are selectively formed. In the crystal, the complex cations and the PF6−anions are connected through weak N—H...F, C—H...F and C—H...S hydrogen bonds into a three-dimensional structure. Two F atoms in one PF6anion are disordered over two sets of sites with refined occupancies of 0.61 (4) and 0.39 (4) and two F atoms in the other PF6−anion are disordered over two sets of sites with occupancies of 0.5.

scholarly journals Crystal structure of ethyl 6-methyl-2-oxo-4-(3,4,5-trimethoxyphenyl)-1,2,3,4-tetrahydropyrimidine-5-carboxylate

2015 ◽  
Vol 71 (3) ◽  
pp. o206-o207 ◽  
Author(s):  
J. J. Novina ◽  
G. Vasuki ◽  
M. Suresh ◽  
M. Syed Ali Padusha
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Three Dimensional ◽  
Dimensional Structure ◽  
Boat Conformation ◽  
Compound C ◽  
Centroid Distance ◽  
The Mean ◽  
Ring Motif

In the title compound, C17H22N2O6, the dihydropyrimidine ring adopts a flattened boat conformation. The dihedral angle between the benzene ring and the mean plane of the dihydropyrimidine ring is 75.25 (6)°. In the crystal, molecules are linkedviapairs of N—H...O hydrogen bonds, forming inversion dimers with anR22(8) ring motif which are linked through N—H...O and weak C—H...O hydrogen bonds. These, together with π–π ring interactions [centroid–centroid distance = 3.7965 (10) Å], give an overall three-dimensional structure.

Synthesis and characterization of 2,2-diphenyl-1-(5-acetonyl-2,4,6-trinitro-1,3-cyclohexadienyl)hydrazine, C21H19N5O7

1993 ◽  
Vol 71 (7) ◽  
pp. 1057-1063 ◽  
Author(s):  
Donna L. Draper ◽  
Richard J. Barton ◽  
Beverly E. Robertson ◽  
Barbara R. Nelson ◽  
John A. Weil
Keyword(s):  
Nitro Group ◽  
Synthesis And Characterization ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Phenyl Rings ◽  
Common Plane ◽  
Twist Boat

The reaction of 2,2-diphenyl-1-(2,4,6-trinitrophenyl)hydrazine with the enolate of acetone, followed by acidification, yields the title compound 2,2-diphenyl-1-(5-acetonyl-2,4,6-trinitro-1,3-cyclohexadienyl)hydrazine, C21H19N5O7. The identity of the latter was confirmed by a combination of mass spectrometry, FTIR, elemental analysis, and 1H NMR. Crystals were grown from dichloromethane –95% ethanol and the structure was determined by X-ray diffraction. Crystals are monoclinic, P21/c, a = 9.254(3), b = 13.531(3), c = 17.39(5) Å, β = 106.18(2)° at 225 K. R = 0.073, Rω = 0.038 for reflections with I > 2σ(I). The Zachariasen extinction factor, g, refined to 18(3) × 10−4. The cyclohexadiene ring is puckered with a primarily twist-boat conformation. Atoms C(1) to C(3), C(6), the nitro group on C(2), and the hydrazine moiety (N(8)—N(7)—H(7) attached to C(1)) all lie close to a common plane. The planes of the two phenyl rings, the acetonyl substituent, and the C(6) nitro group are each roughly perpendicular to this plane. The C(5) acetonyl and C(6) nitro groups are trans to each other.

scholarly journals Crystal structure of 1,2,3,4-di-O-methylene-α-D-galactopyranose

2015 ◽  
Vol 71 (12) ◽  
pp. o961-o962
Author(s):  
Ioannis Tiritiris ◽  
Stefan Tussetschläger ◽  
Willi Kantlehner
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Sodium Methoxide ◽  
Three Dimensional ◽  
Boat Conformation ◽  
Pyranose Ring ◽  
Compound C ◽  
Dimensional Network ◽  
Twist Boat

The title compound, C8H12O6, was synthesized by deacetylation of 6-acetyl-1,2,3,4-di-O-methylene-α-D-galactose with sodium methoxide. The central part of the molecule consists of a six-membered C5O pyranose ring with a twist-boat conformation. Both fused dioxolane rings adopt an envelope conformation with C and O atoms as the flap. In the crystal, O—H...O and C—H...O hydrogen bonds are present between adjacent molecules, generating a three-dimensional network.

Structural and theoretical characterization of a new twisted 4′-substituted terpyridine compound: 4′-(isoquinolin-4-yl)-2,2′:6′,2′′-terpyridine

2016 ◽  
Vol 72 (12) ◽  
pp. 932-938 ◽  
Author(s):  
Juan Granifo ◽  
Beatriz Arévalo ◽  
Rubén Gaviño ◽  
Sebastián Suárez ◽  
Ricardo Baggio
Keyword(s):  
Hydrogen Bonding ◽  
Hydrogen Bonds ◽  
Noncovalent Interactions ◽  
Three Dimensional ◽  
Point Of View ◽  
Donor Atom ◽  
Aim Analysis ◽  
Compound C ◽  
Derivatives Of

4′-Substituted derivatives of 2,2′:6′,2′′-terpyridine with N-containing heteroaromatic substituents, such as pyridyl groups, might be able to coordinate metal centres through the extra N-donor atom, in addition to the chelating terpyridine N atoms. The incorporation of these peripheral N-donor sites would also allow for the diversification of the types of noncovalent interactions present, such as hydrogen bonding and π–π stacking. The title compound, C24H16N4, consists of a 2,2′:6′,2′′-terpyridine nucleus (tpy), with a pendant isoquinoline group (isq) bound at the central pyridine (py) ring. The tpy nucleus deviates slightly from planarity, with interplanar angles between the lateral and central py rings in the range 2.24 (7)–7.90 (7)°, while the isq group is rotated significantly [by 46.57 (6)°] out of this planar scheme, associated with a short Htpy...Hisqcontact of 2.32 Å. There are no strong noncovalent interactions in the structure, the main ones being of the π–π and C—H...π types, giving rise to columnar arrays along [001], further linked by C—H...N hydrogen bonds into a three-dimensional supramolecular structure. An Atoms In Molecules (AIM) analysis of the noncovalent interactions provided illuminating results, and while confirming the bonding character for all those interactions unquestionable from a geometrical point of view, it also provided answers for some cases where geometric parameters are not informative, in particular, the short Htpy...Hisqcontact of 2.32 Å to which AIM ascribed an attractive character.

scholarly journals 1-Ethyl-4-phenyl-1H-1,5-benzodiazepin-2(3H)-one

IUCrData ◽  
2016 ◽  
Vol 1 (4) ◽  
Author(s):  
Abdelhanine Essaghouani ◽  
Younos Bouzian ◽  
El Mokhtar Essassi ◽  
Mohamed Saadi ◽  
Lahcen El Ammari
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Phenyl Ring ◽  
Three Dimensional ◽  
Dimensional Structure ◽  
Boat Conformation ◽  
Ethyl Group ◽  
Bond Forming ◽  
Compound C

The title compound, C17H16N2O, consists of a benzodiazepin-2-one moiety substituted with a phenyl ring and an ethyl group. The seven-membered diazepine ring has a boat conformation and the fused benzene ring is nearly perpendicular to the phenyl ring, as indicated by the dihedral angle of 74.90 (8)°. The atoms of the ethyl group are disordered over two sets of sites, with a refined occupancy ratio of 0.603 (15):0.397 (15). In the crystal, molecules are linked by pairs of C—H...O hydrogen bonds, forming inversion dimers. The dimers are linkedviaa further C—H...O hydrogen bond, forming layers parallel to (001), which are in turn linked by C—H...π interactions, forming a three-dimensional structure.

scholarly journals 1-Allyl-3′-phenyl-6′H-spiro[indoline-3,4′-isoxazolo[4′,5′:5,6]pyrido[2,3-d]pyrimidine]-2,5′,7′(8′H,9′H)-trione dimethyl sulfoxide monosolvate

IUCrData ◽  
2017 ◽  
Vol 2 (1) ◽  
Author(s):  
P. Seethalakshmi ◽  
C. Palanivel
Keyword(s):  
Hydrogen Bonds ◽  
Dimethyl Sulfoxide ◽  
Phenyl Ring ◽  
Solvent Molecule ◽  
Three Dimensional ◽  
Pyrimidine Ring ◽  
Ring System ◽  
Dimensional Structure ◽  
Boat Conformation ◽  
Compound C

In the title solvated compound, C24H17N5O4·C2H6OS, the solvent molecule, dimethyl sulfoxide, is linked to the title molecule by an N—H...O hydrogen bond. The pyridine ring adopts a twist-boat conformation. The isoxazole ring is inclined to the indoline ring system, the pyrimidine ring, and the phenyl ring by 82.31 (7), 10.41 (8) and 53.77 (10)°, respectively. There is an intramolecular C—H...π interaction present involving the phenyl ring and the indoline ring system. In the crystal, molecules are connected by two pairs of N—H...O hydrogen bonds, forming chains along theb-axis direction, and enclosingR22(8) andR22(14) ring motifs. The chains are linked by C—H...O and C—H...N hydrogen bonds and offset π–π interactions, between the pyrimidine and isoxazole rings of inversion-related molecules [centroid–centroid distance = 3.7140 (9) Å], forming a three-dimensional structure.

Synthesis and characterization of two new chiral Kemp’s acid derivatives: structures fixed by a peculiar system of N–H···O, C–H···O and C–H···N hydrogen bonds

2016 ◽  
Vol 231 (9) ◽  
Author(s):  
Richard Pažout ◽  
Jaroslav Maixner ◽  
Jan Pecháček ◽  
Beáta Vilhanová ◽  
Petr Kačer
Keyword(s):  
Hydrogen Bonds ◽  
Asymmetric Reactions ◽  
Synthesis And Characterization ◽  
Catalytic Asymmetric ◽  
Derivatives Of ◽  
Oxazoline Derivatives ◽  
Catalytic Asymmetric Reactions

AbstractNew chiral imide-oxazoline derivatives of Kemp’s acid were synthesized with the aim to produce new ligands suitable for catalytic asymmetric reactions. Compound

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