Synthesis and Crystal Structure of 3-（4-Bromobenzyloxy）-6-morpholinopyridazine

The title compound 3-(4-bromobenzyloxy)-6-morpholinopyridazine(C15H16BrN3O2) was synthesized,and its crystal structure was studied.It crystallizes in the triclinic system,space group P with a = 8.3408(17),b = 8.8620(18),c = 10.832(2) ,α = 108.09(3),β = 91.28(3),γ = 100.90(3)°,Dc = 1.562 g/cm3,Z = 2,λ = 0.71073 ,μ(MoKα) = 2.769 mm-1,Mr = 350.22,V = 744.5(3) 3,F(000) = 356,the final R = 0.0522 and wR = 0.1366 for 2016 observed reflections with I > 2σ(I).In the crystal structure,the morpholine ring adopts a chair conformation with O(2) and N(3) atoms at the flap positions-0.656(7) and 0.622(6)  out of the mean plane formed by the other four C atoms,respectively.These molecules generate centro-symmetric dimers through intermolecular π-π interaction.     

Synthesis and Crystal Structure of 2-(4’-Methylphenoxy)-5,8,9-trimethyl-3-phenyl Thieno[3′,2′:5,6]pyrido[4,3-d]pyrimidin-4-(3H)-one Hydrochloride

1 INTRODUCTION Pyrido[4,3-d]pyrimidine derivatives have pharma- ceutical activity and germicidal action[1~3]. So far, hundreds of tetrahydro- and octahydro-pyrido[4,3- d]pyrimidines have been synthesized as potential diuretic, antirheumatic and bacteriostatic drugs, but only a few of fully aromatic pyrido[4,3-d] pyrimi- dines are known. An important synthetic route to synthesize fully aromatic pyrido[4,3-d]pyrimidines is the condensation reaction of 4-aminonicotinic acid and amines[4]. Ho…     

Synthesis,Bioactivity and Crystal Structure Analysis of N-（2-ethoxyphenyl）-3-oxobenzo[d]isothiazole-2（3H）-carboxamide

The title compound N-(2-ethoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxa-mide(C16H14N2O3S,Mr = 314.35) has been synthesized and structurally characterized by IR,1H NMR and single-crystal X-ray diffraction.The crystal belongs to triclinic,space group P with a = 4.6395(15),b = 8.689(3),c = 17.917(7),α = 87.763(9),β = 84.625(9),γ = 82.344(9)°,V = 712.4(4)3,Z = 2,Dc = 1.465 Mg·m-3,λ(MoKa) = 0.71073,F(000) = 328,μ(MoKa) = 0.242 mm-1,the final R = 0.038 and wR = 0.089.A total of 3702 unique reflections were collected,of which 2762 with I > 2σ(I) were observed.X-ray analysis revealed that the benzisothiazolone ring and benzene moieties were essentially planar,and three intramolecular hydrogen bonds N(2)-H(2N)…O(1),N(2)-H(2N)…O(3) and C(10)-H(10)…O(2) were observed.The preliminary biologi-cal test showed that the title compound had antifungal and antibacteria activities against Bacillus subtilis(CMCC63003),Aeromonas hydrophila(ATCC7966),Staphylococcus aureus(ATCC6538),Escherichia coli(JM103),Blastomyces albicans,Gloeosporium papaya P.Henn,Colletotrichum gloeosporioides Penz and Botryodiplodia theobromae.     

Synthesis,Bioactivity and Crystal Structure Analysis of Novel Benzo[d]isothiazol-3（2H）-ones

Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2(3H)-carboxamide (1) and N-(2-methoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxamide (2),were synthesized from the initial compound benzo[d]isothiazol-3(2H)-one (BIT) and characterized by 1 H NMR,IR and elemental analysis,respectively.The single crystals of compounds 1 and 2 were obtained and determined by X-ray diffraction analysis.The preliminary results of biological activity experiment show that some of the title compounds exhibited a favorable antimicrobial activity.     

Synthesis and Crystal Structure of 1,2-Dis（1,3-diphenylpropan-2-yl）disulfane

A novel compound of 1,2-dis(1,3-diphenylpropan-2-yl)disulfane(C30H30S2,Mr=454.27)was synthesized in ethanol with 1,3-diphenyl-2-propanone as raw materials,giving high yield of product(90%).Its structure was determined by IR,1H NMR,MS,elemental analysis and X-ray diffraction.The crystal belongs to monoclinic,space group C2 with a=18.727(3),b=6.5179(9),c=13.7576(18),β=131.0610(10)o,V=1266.2(3)3,Z=2,Dc=2.136 g/cm3,μ=1.078 mm-1,F(000)=843,R=0.0490 and wR=0.1247 for 3211 observed reflections with I>2(I).X-ray analysis reveals that the molecule is not symmetrical.There exist no classical hydrogen bonds andπ-πstacking interactions.Moreover,the thermal stability of compound 3 was investigated.     

Synthesis and Crystal Structure of 4,5-Bis（2-chloroethylthio）phthalonitrile

A novel phthalonitrile compound,[C12H10Cl2N2S2],has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 10.6417(8),b = 7.5737(6),c = 18.2758(14),β = 105.2480(10)°,Mr = 317.24,V = 1421.12(19)3,Z = 4,Dc = 1.483 g/cm3,F(000) = 648,μ = 0.733 mm-1,R = 0.0173 and wR = 0.2183.In the structure,the C atoms of the aromatic ring,the two cyanide groups and the two S atoms are almost coplanar(maximum deviation from the mean plane = 0.049(7) ).Two potential weak intermolecular interactions of C-H…N and one type of π…π stacking interaction with a centroid-centroid separation of 3.751(8) stabilize the crystal structure.     

Synthesis and Crystal Structure of 3,3＇-（4-Dimethylaminobenzylidene）- bis-（4-hydroxycoumarin）

The title compound 3,3'-(4-dimethylaminobenzylidene)-bis-(4-hydroxycoumarin) 3 was synthesized by the reaction of 4-hydroxycoumarin with 4-dimethylaminobenzaldehyde, and its chemical structure was determined by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P21/n with a = 11.698(2), b = 10.882(2), c = 16.594(3) , β = 90.69(3)o, V = 2112.1(7) 3, Z = 4, F(000) = 952, Dc = 1.432 Mg/m3, Mr = 455.45, μ = 0.102 mm-1, λ = 0.71073 , the final R = 0.0779 and wR = 0.2143 for 3031 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of 2-Nitro-9,9-bis（methylpropionate）fluorine

The title compound of 2-nitro-9,9-bis(methylpropionate)fluorine (C21H21NO6 , Mr=383.39) was synthesized for the first time. Complete assignments were achieved by 1H NMR, IR, EI-MS, elemental analysis and single-crystal X-ray diffraction technique. The crystal belongs to monoclinic, space group P21/c with a=11.4581(15), b=10.3624(14), c=16.573(2) , β=96.629(2) o , V=1954.6(5) 3 , Z=4, Dc=1.303 g/cm 3 , μ=0.096 mm -1 , F(000) = 808, R =0.0493 and wR=0.1499 for 3107 observed reflections with I > 2σ(I). X-ray analysis reveals that three fused rings of the fluorene system are almost coplanar and the two ester groups are nearly perpendicular to the fused-ring system. Weak C-H O hydrogen bonding connects the molecules into centrosymmetric dimmers.     

Synthesis and Crystal Structure of 9-（4-Dimethylaminophenyl）-l,8-dioxo- 9H-dibenzo [c,h ]-2,7,10-trioxanthene

The title compound 9-(4-dimethylaminophenyl)-1,8-dioxo-9H-dibenzo[c,h]- 2,7,10-trioxanthene (3) was synthesized by the reaction of 4-hydroxycoumarin with 4-dimethyla- minobenzaldehyde, and its chemical structure was determined by X-ray single-crystal diffraction. It crystallizes in triclinic, space group P with a = 7.8753(16), b = 11.029(2), c = 12.913(3) , α = 69.79(3), β = 89.01(3), γ = 81.90(3)°, V = 1041.5(4) 3, Z = 2 , F(000) = 456, Dc = 1.395 Mg/m3, Mr = 437.43, μ = 0.097 mm-1, λ = 0.71073 , the final R = 0.0491 and wR = 0.1314 for 2662 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of （E）-N,N＇- dicyclohexyl- 1-（3-（3,4-dihydroxyphenyl）acryloyl）urea

The title compound, (E)-N,N′-dicyclohexyl-1-(3-(3,4-dihydroxyphenyl)acryloyl)- urea (DDA), has been synthesized and characterized by FT-IR and 1H-NMR spectroscopy, ESI- MS, and X-ray single-crystal diffraction. Its crystallizes in monoclinic, space group C2/c with a = 20.483(12), b = 11.153(6), c = 21.134(12) , β = 117.098(7), V = 4298(4) 3, Z = 8, F(000) = 1664, Dc = 1.195 Mg/m3, Mr = 386.48, μ= 0.082 mm-1, the final R = 0.0474 and wR = 0.1370 for 4853 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of 8-Methyl-7-（3-nitrophenyl）-10-phenyl-10,11-dihydrochro-meno[4,3-b]pyrazolo[4,3-e]pyridin-6-（7H）-one

The title compound(C26H18N4O4) has been synthesized via a three-component reaction and it was characterized by means of IR and 1H NMR.Its crystal and molecular structures were determined by X-ray diffractometry.It belongs to the triclinic system,space group P1 with a = 7.7288(15),b = 11.168(2),c = 12.645(3) ,α = 107.02(3),β = 90.85(3),γ = 101.93(3)°,V = 1017.9(3) 3,Mr = 450.44,Z = 2,Dc = 1.470 g/cm3,λ = 1.54178 ,μ = 0.836 mm-1,F(000) = 468,the final R = 0.0488 and wR = 0.1180.A total of 11903 reflections were collected,of which 3642 were independent(Rint = 0.0377) and 3025 were observed with I > 2σ(I).     

Synthesis and Crystal Structure of 2,3,4,6-tetra-O-Acetyl-1-{4-chloro-3-[1-（4-ethoxyphenyl）-1-methylethyl]phenyl}-1-deoxy-β-D-glucopyranose

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic system(C31H37ClO10,Mr = 605.06),space group P21 with a = 11.882(5),b = 10.106(5),c = 13.816(6),V = 1545.9(12)3,Z = 2,Dc = 1.300 g/cm3,F(000) = 640,μ = 0.179 mm-1,the final R = 0.0430 and wR = 0.0595 for 4960 observed reflections(I > 2σ(I)).The title compound was confirmed to be a β-anomer by single-crystal X-ray diffraction and 1H NMR.The proximal benzene ring is nearly orthogonal to the glucopyranoside ring,and the two benzene rings are also almost orthogonal to each other.Four non-classical intermolecular hydrogen bonds observed in the crystal lattice help to stabilize the crystal.     

Synthesis and Crystal Structure of （E）-Ethyl 3-Keto-18β-glycyrrhetinate 3-Oxime

A novel derivative of glycyrrhetinic acid, (E)-ethyl 3-keto-18β-glycyrrhetinate 3- oxime C32H49NO4 (Mr = 511.72), was synthesized and structurally characterized by IR, 1H NMR and single-crystal X-ray diffraction. It belongs to monoclinic, space group P21, with a = 12.4897(12), b = 7.3190(7), c = 15.9944(14) , β = 94.833(2)o, V = 1456.9(2) 3, Z = 2, Dc = 1.167 g/cm3, μ = 0.075 mm-1, F(000) = 560, the final R = 0.0449 and wR = 0.1122. A total of 7486 reflections were collected, of which 2785 were independent (Rint = 0.0199) and 2605 were observed with I > 2σ(I). There exists an intermolecular hydrogen bond which helps to stabilize the crystal structure.     

Synthesis and Crystal Structure of N-（（6-chloropyridin-3-yl）methyl）-6-ethoxy-N-ethyl-3-nitropyridin-2-amine

The title compound N-((6-chloropyridin-3-yl)methyl)-6-ethoxy-N-ethyl-3-nitropyri-din-2-amine(4) was synthesized by reacting the mixture of 6-chloro-2-ethoxy-3-nitropyridine(1) and 2-chloro-6-ethoxy-3-nitropyridine(2) with 3,and its structure was determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 7.3441(2),b = 9.9041(3),c = 11.7368(3) ,α = 101.410(2),β = 102.1340(10),γ = 99.594(2)o,μ = 0.260 mm-1,Mr = 336.78,V = 798.58(4)3,Z = 2,Dc = 1.401g/cm3,F(000) = 352,T = 296(2) K,R = 0.0210 and wR = 0.1053.     

Microwave Synthesis and Crystal Structure of Bis {2- [（2,4-dichloro-phenylimino）- methyl]-4,6-diiodo-phenol}-copper（II）

Bis{2-[(2,4-dichloro-phenylimino)-methyl]-4,6-diiodo-phenol}-copper(II) (1) has been synthesized and its structure determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P2 1 /n with a=14.7558(17), b=20.770(2), c=20.3260(19) , β=90.6110(10)°, V=6229.2(11) 3 and Z=8. The Cu atom is surrounded by two O atoms and two N atoms from two 2-[(2,4-dichloro-phenylimino)-methyl]-4,6-diiodo-phenol molecules to form a tetrahedral coordination environment. The complex is linked into a column by weak intermolecular interactions.     

Synthesis and Crystal Structure Analysis of 5′-O-Tosyl-2,3′-anhydrothymidine

In this paper=5′-O-tosyl-2,3′-anhydrothymidine has been synthesized and its crystal structure was analyzed. The crystal belongs to the triclinic system=space group P1=with a=5.397(2)=b=6.1886(18)=c=3.507(5) =α =87.74(2)=β =89.84(4)=γ =73.79(2)°=C17H18N2O6S=Mr=378.39=Z=1=V=432.8(3)3=Dc=1.452 g/cm3=F(000)=198 and Flack =-0.11(14). No intermolecular hydrogen bonds exist in the crystal=and the angle between benzene ring and pyrimidine planes is 32.23°.     

Synthesis, Characterization and Crystal Structure of （＋）-N-[（3S）-3-（4- fluoroph enyl）heptan oyl] bornan e-10,2-s ultam

The chiral molecule (+)-N-[(3S)-3-(4-fluorophenyl)heptanoyl]bornane-10,2-sultam (C23H32FNO3S, Mr = 421.56), a fluorine-containing derivative of camphorsultam, was conveniently obtained and crystallized in the orthorhombic space group P212121 with a = 7.9044(11), b = 11.6680(16), c = 24.899(3) , V = 2296.4(5) 3, Z = 4, Dc = 1.219 Mg/m3, λ = 0.71073 , μ(MoKα) = 0.172 mm-1 and F(000) = 904. X-ray diffraction analysis reveals that the six-membered ring of sultam shows a boat conformation (Fig. 1). The planes constructed by ((C6), (C7), (C8), (C9)) and ((C4), (C5), (C6), (C9)) form a dihedral angle of 70.3(3)°. The plane of (C1)-(C2)-(C3) forms dihedral angles to the aforementioned planes of 85.9(4) and 89.5(4)°, respectively. The molecules are linked via C-H···O/F interactions.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Cobalt（Ⅱ） Complex

A metal-organic coordination polymer [Co2(cbba)4(bix)2]n(Hcbba = 2-(4'-chlorine-benzoyl)-benzoic acid,bix = 1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis,IR,TG,and single-crystal X-ray diffraction.Pink crystals crystallize in the monoclinic system,space group P21/n with a = 21.148(4),b = 15.728(3),c = 23.879(4) ,β = 102.148(3)°,V = 7764(2)3,C316H232Cl15Co8N32O48,Mr = 6248.53,Dc = 1.336 g/cm3,F(000) = 3207,Z = 1,μ(MoKα) = 0.621 mm-1,the final R = 0.0567 and wR = 0.1280 for 8510 observed reflections(I > 2σ(I)).The structure of 1 exhibits a one-dimensional chain-like structure.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Cadmium（Ⅱ） Complex

A metal-organic coordination polymer [Cd2(cbba)4(bix)2] n·nH2O (Hcbba=2-(4′-chlorine-benzoyl)-benzoic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Colorless crystals crystallize in the triclinic system, space group Pī with a=12.9891(15), b=15.3211(19), c=21.154(3), α=108.476(3), β=90.148(2), γ=105.429(3)°, V=3831.5(8)3 , C84H60Cd2Cl4N8O13 , Mr=1756.00, Dc=1.522g/cm3 , F(000)=1776, Z=2, μ(MoKα)=0.765 mm-1 , the final R=0.0724 and wR=0.1208 for 6916 observed reflections (I > 2σ(I)). The structure of 1 exhibits a one-dimensional infinite chain-like structure.