1D and 2D NMR studies of 2–(2–(BENZYLOXY)–3–METHOXYPHENYL)–1H–BENZIMIDAZOLEF

The reaction of Benzyl o–vanillin 1 and o–phenylene diamine 2 in dichloromethane produced new benzimidazole, 3. The complete assignments of 3 were made using 1D and 2D NMR including COSY, HMQC and HMBC NMR in CDCl3 and acetone–d6. The coupling constants J are reported in Hertz, and the differences in the peak splittings using both solvents are discusse

1D and 2D NMR studies of BENZYL O–VANILLIN

The reaction of o–vanillin A with benzyl bromide B2 in acetone as the solvent and K2CO3 as a base in the presence of tetra–n–butylammonium iodide (TBAI) as catalyst formed benzyl o–vanillin, C. The complete assignments of C using PROTON, APT, DEPT–135, COSY, NOESY, HMQC and HMBC NMR in both CDCl3 and acetone–d6 are discussed, and the coupling constants J are reported in Hertz (Hz)

1,3-Oxazepane-4,7-Diones Compounds: 1Hand 13CNMR High-Resolution Spectroscopy (1D and 2D)

“Oxazepine” refers to any seven-membered ring containing an oxygen and nitrogen atom. The 1,3-oxazepine is a branch of many types of the heterocyclic oxazepine [1–7]. The core structure of 1,3-oxazepane-4,7diones consists of a sevenmemebred ring along with two carbonyl group. Over the years, the syntheses of oxazepine derivatives have been investigated and documented. The result is important of heterocyclic compounds having significant biological uses [8– 13]. Recently, we prepared a variety of 1,3-oxazepinediones in order to study the spectroscopic and liquid crystal properties [14]. In this paper, we present the structural elucidation by 1D and 2D NMR experiments of 3-alkyl- 2-(3-hydroxyphenyl)-1,3-oxazepane-4,7-diones with general formula(HOC6H4)CONCnH2n+1CH-CH(CO)2 (where n = 2, 4, 6, 8, 10, 12, 14, 16, and 18). Here, the hydroxyphenyl and the terminal alkyl chain are attached to the oxazepane ring

Ethyl 1-(2-hy­droxy­eth­yl)-2-(4-meth­oxy­phen­yl)-1H-benzimidazole-5-carboxyl­ate monohydrate

In the title mol­ecule, C19H20N2O4·H2O, the benzimidazole ring system is essentially planar [maximum deviation = 0.013 (11) Å] and is inclined to the 4-meth­oxy­phenyl ring by 30.98 (5)°. In the crystal, O—H⋯O and O—H⋯N hydrogen bonds involving the water mol­ecule link neighbouring mol­ecules, forming a two-dimensional network lying parallel to the bc plane. There are also C—H⋯π and π–π inter­actions present. The latter involve inversion-related benzimidazole rings with centroid–centroid distances of 3.5552 (8) and 3.7466 (8) Å

(3E,5E)-3,5-Bis(naphthalen-1-yl­methyl­idene)piperidin-4-one

In the title compound, C27H21NO, the piperidine ring adopts a chair conformation. The mean plane through the piperidine ring makes dihedral angles of 49.27 (5) and 63.07 (5)° with the naphthalene ring systems. In the crystal, mol­ecules are linked into dimers via pairs of inter­molecular C—H⋯O inter­actions, generating ten-membered R 2 2(10) ring motifs. C—H⋯π inter­actions further stabilize the crystal structure

(E)-6-Bromo-3-{2-[2-(2-meth­oxy­benzyl­idene)hydrazin­yl]-1,3-thia­zol-4-yl}-2H-chromen-2-one

In the title compound, C20H14BrN3O3S, the mol­ecule adopts an E configuration about the central C=N double bond. The chromene ring system and the thia­zole ring are approximately planar [maximum deviations = 0.029 (3) and 0.007 (3) Å, respectively]. The chromene ring system is inclined at angles of 7.37 (12) and 13.90 (13)° with respect to the thia­zole and benzene rings, respectively, while the thia­zole ring makes a dihedral angle of 12.58 (15)° with the benzene ring. In the crystal, mol­ecules are connected by N—H⋯O hydrogen bonds, forming C(8) supra­molecular chains along the c axis

5-[(E)-Benzyl­idene]-2-hy­droxy-10-methyl-8-phenyl-3,10-diazahexa­cyclo­[10.7.1.13,7.02,11.07,11.016,20]henicosa-1(19),12(20),13,15,17-pentaen-6-one ethanol 0.25-solvate 0.6-hydrate

In the title compound, C33H28N2O2·0.25C2H6O·0.6H2O, the piperidone ring adopts a chair conformation and the pyrrolidine ring adopts an envelope conformation. The dihedral angle between the two phenyl rings is 70.83 (16)°. One of the N atoms of the organic mol­ecule is disordered over two positions in a 0.52 (4):0.48 (4) ratio and the two solvent mol­ecules are partially occupied and show high displacement parameters. In the crystal, mol­ecules are connected by inter­molecular O—H⋯O and C—H⋯O hydrogen bonds, forming a three-dimensional network

(E)-6-Bromo-3-{2-[2-(2-chloro­benzyl­idene)hydrazin­yl]thia­zol-5-yl}-2H-chromen-2-one dimethyl sulfoxide monosolvate

In the title compound C19H11N3O2SClBr·C2H6OS, the mol­ecule adopts an E configuration about the central C=N double bond. The chromene ring system and the thia­zole ring are approximately planar, with maximum deviations of 0.027 (2) and 0.003 (1) Å, respectively. The central thia­zole ring makes dihedral angles of 21.82 (9) and 5.88 (7)° with the chloro-substituted phenyl ring and the chromene ring, respectively. In the crystal, mol­ecules are connected via N—H⋯O, N—H⋯S and C—H⋯O hydrogen bonds, forming supra­molecular chains along the c axis. An intra­molecular C—H⋯O hydrogen bond occurs. π–π inter­actions are observed between the thia­zole and phenyl rings [centroid–centroid distance = 3.6293 (10) Å]. A short Br⋯Cl contact of 3.37 (6) Å also occurs

4-Methyl-2-oxo-2H-chromen-7-yl 4-fluoro­benzene­sulfonate

In the asymmetric unit of the title compound, C16H11FO5S, the 2H-chromene ring is essentially planar, with a maximum deviation of 0.040 (2) Å. The dihedral angle between the 2H-chromene ring and the 4-fluoro­phenyl ring is 2.17 (8)°. One of the sulfonamide O atoms is approximately coplanar with the benzene ring [C—C—S—O torsion angle = 166.00 (14)°], whereas the other O atom lies well below the plane [C—C—S—O = −61.35 (17)°]. In the crystal, mol­ecules are connected by weak C—H⋯O hydrogen bonds, forming two-dimensional networks parallel to the ac plane

(E)-3-(2-{2-[1-(3-Hy­droxy­phen­yl)ethyl­idene]hydrazin­yl}-1,3-thia­zol-4-yl)-2H-chromen-2-one

In the title compound, C20H15N3O3S, the thia­zole ring is approximately planar, with a maximum deviation of 0.003 (1) Å, and makes dihedral angles of 7.44 (6) and 1.88 (6)° with the hy­droxy-substituted phenyl ring and the pyran ring, respectively. The hydroxyl group is disordered over two sets of sites, with an occupancy ratio of 0.567 (3):0.433 (3). In the crystal, the major disorder component mol­ecules are connected via bifurcated (three-centre) O—H⋯O and C—H⋯O hydrogen bonds, generating R 1 2(6) motifs and resulting in supra­molecular chains along the a axis. In the minor occupancy component, however, mol­ecules are connected via C—H⋯O hydrogen bonds, forming supra­molecular chains along the b axis. Furthermore, the crystal structure is stabilized by π–π inter­actions between the thia­zole rings [centroid–centroid distance = 3.5476 (7) Å]