Synthesis and Crystal Structure of 9-（2-Hydroxy-5-nitrophenyl）-9H-dibenzo[c,h]-2,7,10-trioxanthene-1,8-dione DMF Solvate

The title compound 9-(2-hydroxy-5-nitrophenyl)-9H-dibenzo[c,h]-2,7,10-trioxan-thene-1,8-dione DMF solvate (C28H20N2O9,Mr=528.46) was synthesized and crystallized.The crystal belongs to the triclinic system,space group P1 with a=10.210(3),b=10.698(4),c=12.522(4),α=92.214(6),β=113.751(5),γ=105.040(5)°,Z=2,V=1193.0(7)3,Dc=1.471 g·cm-3,μ(MoKα)=0.112 mm-1,F(000)=548,R=0.0444 and wR=0.1141 for 2667 observed reflections (I 2σ(I)).X-ray analysis reveals that atoms C(1),C(2),C(3),C(4),C(5) and O(1) on the new 4H-pyran ring are slightly distorted,forming a half-chair conformation.     

Synthesis and Crystal Structure of 5-Cyclopropyl- 10-（4-fluorophenyl）-7,7-dimethyl-7,8-dihydro-5H- indeno[1,2-b]quinoline-9,11（6H,10H）-dione

The title compound 5-cyclopropyl-10-(4-fluorophenyl)-7,7-dimethyl-7,8-dihydro- 5H-indeno[1,2-b]quinolne-9,11(6H,10H)-dione was obtained by the reaction of 4-fluorobenzal- dehyde, 2H-indene-1,3-dione and 3-(cyclopropylamino)-5,5-dimethylcyclohex-2-enone in the presence of acetic acid under microwave irradiation. Its structure was confirmed by IR and 1H- NMR spectra. The crystal is of monoclinic, space group P21/c with a = 14.138(3), b = 8.952(2), c = 17.140(3) , β = 102.253(3)o, C27H24FNO2, Mr = 413.47, Z = 4, V = 2119.9(8) 3, Dc = 1.296 g/cm3, μ(MoKα) = 0.087 mm-1, F(000) = 872, the final R = 0.0425 and wR = 0.0905 for 2336 observed reflections (I > 2σ(I)). X-ray analysis revealed that the pyridine ring adopts a boat conformation and the six-membered ring fused with it assumes a twist boat conformation.     

Synthesis and Crystal Structure of 9-Amino-7-（2-chlorophenyl）-6H-benzo[c]thiochromene-8,8,10（7H）-tricarbonitrile DMF Solvate

The title compound 9-amino-7-(2-chlorophenyl)-6H-benzo[c]thiochromene-8,8,10(7H)-tricarbonitrile DMF solvate(C25H20ClN5OS,Mr = 473.97) was synthesized and crystallized.The crystal belongs to triclinic,space group P1 with a = 7.6393(2),b = 10.5212(3),c = 15.0573(4) ,α = 86.797(1),β = 79.445(1),γ = 75.379(1)°,Z = 2,V = 1151.16(5) 3,Dc = 1.367 g.cm-3,μ(MoKα) = 0.285 mm-1,F(000) = 492,R = 0.0389 and wR = 0.1005 for 3455 observed reflections(I > 2σ(I)).X-ray analysis reveals that the new six-numbered ring(C(1)-C(6)) forms a skew boat conformation.The molecule links a molecule of DMF via the N(1)-H(1A)...O(1) hydrogen bond,while another hydrogen bond C(23)-H(23A)...N(2) links adjacent molecules,forming dimmers along the a axis.     

Synthesis and Crystal Structure of exo-4-（3,4-Dichlorophenyl）-8-ethyl-3,3a,4,5,8, 12d-hexahydro-2H-furo[3,2-c]indolo[3,2-f]quinoline

The title compound exo-4-(3,4-dichlorophenyl)-8-ethyl-3,3a,4,5,8,12d-hexahydro-2H-furo[3,2-c]indolo[3,2-f]quinoline (C25H22Cl2N2O, Mr = 437.35) was synthesized and crystallized. The crystal belongs to tetragonal, space group I4(1)/a with a = 17.4903(3), b = 17.4903(3), c = 28.3403(5) , Z = 16, V = 8669.6(3) 3, Dc = 1.340 g·cm-3, μ(MoKɑ) = 0.319 mm-1, F(000) = 3648, R = 0.0429 and wR = 0.711 for 2714 observed reflections I > 2σ(I). X-ray analysis reveals that atoms C(1), C(2), C(3), C(4), C(5) and N(1) on the new pyridine ring are slightly distorted, forming a distorted boat conformation.     

Synthesis and Crystal Structure of 5-（p-Toly1）-4- [2-（2,4-dichlorophenoxy）acetamido]-l,2,4- triazole-3-thione Ethyl Acetate Solvate

A novel compound 5-（p-tolyl）-4-[2-（2,4-dichlorophenoxy）acetamido]-1,2,4-tria zole- 3-thione 2a has been synthesized by the reaction of 5-（p-tolyl）-4-amino-1,2,4-triazole-3-thione 1 with 2-（2,4-dich/orophenoxy）acetyl ch/oride. Interestingly, the title compound 2 was obtained when 2a crystallizes from a mixed solution of petroleum ether and ethyl acetate, and it has been characterized by elemental analysis, IR, ^1H NMR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 9.780（5）, b = 10.876（6）, c = 11.615（6） /A, a = 104.822（7）, β= 94.105（6）, ）, = 94.305（6）°, V= 1185.7（11）/A3, Z = 2,μ = 0.397 mm^-1, Mr= 497.39, Dx= 1.393 g/cm^3, F（000） = 516, S = 1.097, the final R = 0.0730 and wR = 0.2133 for 4111 unique reflections （Rint = 0.0525） with 3212 observed ones. The dihedral angles made by the triazole ring with the methyl- and chloro-substituted benzene rings are 43.5（7） and 50.2（9）°, respectively. Some intra- and intermolecular hydrogen bonds together with C-H…π interactions existing in the lattice stabilize the crystal structure.     

Synthesis and Crystal Structure of 3-（2,4-Dichlorophenyl）- 4-dydroxy-5-cyclohexanyl-△3-dihydrofuran-2-one

The title compound 3-（2,4-dichlorophenyl）-4-dydroxy-3-（2,4-dichlorophenyl）-4- dydroxy-5-cyclohexanyl-A3-dihydrofuran-2-one 5 has been synthesized by the cyclization of methyl O-（2,4-dichlorophenyl-acetyl）-1-hydroxycyclo-hexane-carboxylate 4, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.8192（3）, b = 10.5053（5）, c = 10.5811（5）A,α = 71.681（10）, β = 78.905（12）, γ = 81.036（12）°, C15H14C1203, Mr = 313.18, V= 702.44（6）A3, Z = 2, De= 1.481 g/cm^3, F（000） = 324,μ = 0.465 mm^-1, S = 1.006, the final R = 0.0331 and wR = 0.1363 for 2505 observed reflections with I 〉 2σ（I） and 183 variable parameters. The crystal analysis shows that the cyclohexene unit of the title compound has a quasi-chair conformation, and a one-dimensional chain structure is formed via the intermolecular hydrogen bond O（1）-H（101）…O（2）.     

Synthesis and Crystal Structure of 3,7,7-Trimethyl- 1-phenyl-4-（3-nitrophenyl）- 4,5,6,7,8,9-hexahydro-1H-pyrazolo [3,4-b]quinoline-5（6H）-one

The title compound (C25H24N4O3) has been prepared by the cyclocondensation of 5-amino-3-methyl-l-phenypyrazol, m-nitrobenaldehyde and dimedone in glycol under microwave irradiation without catalyst. The crystal structure was determined by single-crystal X-ray diffraction to be orthorhombic, space group Pbca with a=16.3331(10), b=13.8329(9), c=19.4163(12) A, V= 4386.8(5)A3, Z=8, Dc=1.298g/cm^3,μ=0.087 mm^-1, F(000)=1808, Mr=428.48, the final R=0.0519 and wR=0.1019. X-ray analysis revealed that the pyridine ring is of boat conformation and the six-membered ring fused with it adopts twist boat conformation.     

Synthesis and Crystal Structure of N-phenyl-N-[（o-nitrophenylacetyl）oxy]benzamide

The compound N-phenyl-N-[（o-nitrophenylacetyl）oxy]benzamide （C21HI6N2Os, Mr = 376） has been synthesized by the reaction of N-hydroxy-N-phenylbenzamide with 2-（2-nitro- phenyl）acetyl chloride in dichlorom-ethane and its structure Was characterized by 1H NMR, 13C NMR, IR, H RMS（ESI） and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group C2/c with a = 32.30（2）, b = 8.400（5）, c = 15.099（9） A, fl = 114.256（10）°, V = 3735（4） A3, Z = 8, D, = 1.339 g/cm3, F（000） = 1568, p = 0.097 mm-1, the final R = 0.0506 and wR = 0.1176 for 2318 observed reflections （1 〉 2a（/））. The title molecule contains three branched chains with its center placed at the midpoint of N. The phenyl ring （C（1）＇-C（6）） makes a dihedral angle of 70.3（1）° with the phenyl ring （C（10）-C（15）） of benzoyl group, and 14.3（1）° with the phenyl ring （C（16） - C（21））, Hydrogen bonds C（5）-H（5）...O（1） and C（12）-H（12）...O（3） together with it-Jr stacking interactions contribute to the stability of the structure.     

Synthesis and Crystal Structure of β-Diketiminate Ytterbium Dichloride

1 TRODUCTIINON The monoanionic b-diketiminato ligands, [ArNC(R)CHC(R)NAr]- [1], are ideal for use with metals and have been applied for early[2] and late[3] transition metals and group 13 metal complexes[4]. These ligands have several attractive feature…     

Synthesis and Crystal Structure of 4-（4-Bromophenyl）- 3,4-dihydro-6-methyl quinolin-2（1H）-one

The title compound (C16H14BrNO) has been synthesized by the reaction of p-tolylamine, Meldrum’s acid and 4-bromo-benzaldehyde, and its structure was characterized by IR, 1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a = 7.6850(11), b = 8.3004(11), c = 21.301(3) , β = 95.110(2)°, V = 1353.4(3) 3, Mr = 316.19, Z = 4, Dc = 1.552 g/cm3, μ(MoKα) = 3.028 mm-1, F(000) = 640, the final R = 0.0345 and wR = 0.0768. X-ray analysis reveals that the atoms of C(1), C(2), C(3), C(4), C(5) and N(1) form a six-membered ring of boat conformation.     

Synthesis of 1,2,3,4,6,7,8,9-octahydropyrimido[4,5-b]quinoline-2,4-dione

In the presence of hydrazine hydrate or sodium ethylate, ethyl 2-[(N-phenylcarbamoyl)amino]-5,6,7,8-tetrahydroquinoline-3-carboxylate is converted to 3-amino- or 3-phenyl-1,2,3,4,6,7,8,9-octahydropyrimido[4,5-b]quinoline-2,4-dione. Compounds analogous to the latter are also obtained during heating of 2-amino-5,6,7,8-tetrahydroquinoline-3-carboxylic arylamides with phenyl isocyanate or from their N-phenylcarbamoyl derivatives.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 8, pp. 1114–1117, August, 1989.     

Synthesis and Crystal Structure of 7-Amino-2,3,4,5-tetrahydro- 1,3-dimethyl- 5-（2-nitrophenyl）-2,4-dioxo-lH-pyrano[2,3- d]pyrimidine-6-carbonitrile DMF Solvate

The title compound 7-amino-2,3,4,5-tetrahydro-1,3-dimethyl-5-（2-nitrophenyl）- 2,4- dioxo-1H-pyrano[2,3-d] pyrirnidine-6-carbonitrile DMF solvate 1 （C19H20N6O6, Mr = 428.41） was synthesized and crystallized. The crystal belongs to the monoclinic system, space group P2 1/c with a = 11.383（2）, b = 13.372（2）, c = 13.673（2）A, β = 97.380（4）°, Z = 4, V = 2063.8（6）A^3, Dc = 1.379 g/cm^3,μ（MoKα） = 0.105 mm^-1, F（000） = 896, the final R = 0.0738 and wR = 0.1647 for 2964 observed reflections （I〉 2σ（I））. X-ray analysis reveals that the new pyran ring is coplanar, which is obviously different from those of other similar compounds. In addition, the unclassical hydrogen bonds of C-H…O and C-H…N are presented in the crystals except for the normal hydrogen bonds of N-H…O.     

3－苯氧甲基－6－（2，4－二氟苯基）－7H-1,2,4-三唑并[3,4-b][1,3,4]噻二嗪的合成与晶体结构研究

由苯氧乙酸出发，经多步反应，制得3-苯氧甲基－4－氨基－5－巯基－1，2， 4－三唑，它与2-氯－2'，4'－二氟苯乙酮进行环化反应，生成3-苯氧甲基－6－（ 2,4-二氟苯基）－7H-1,2,4-三唑并[3,4-b][1,3,4]噻二嗪，通过元素分析、红外 光谱、核磁共振氢谱与碳谱、质谱进行表征，并利用单晶X射线衍射法测定其结构 。晶体属单斜晶系、P2_(1/c)空间群，a = 1.339(3) nm, b = 1.4683(4) nm, c = 0.8606(2) nm, β = 108.49(2)°, Z = 4, F(000) = 736, R_1 = 0.0509。还 对均三唑并噻二唑两类稠杂环的晶体结构作了比较。     

[Zn(DMF)6]H2SiW12O40·(CH3)2NH的合成,晶体结构及性质

The title compound [Zn(DMF)₆]H₂SiW₁₂O₄₀·(CH₃)₂NH was synthesized in mixed solvent of aqueous and acetonitrile, and its crystal structure had been determined using single crystal X-ray diffraction. The crystal belongs to monoclinic, space group C2/m, a=2.0654(4)nm, b=1.3306(3)nm, c=1.3194(3)nm, β=119.59(3)°, V=3.1531(11)nm³, D_c=3.606Mg·m^-3, Z=2, R=0.0462, R_w=0.0836. The title compound comprises of a [Zn(DMF)₆]²⁺ unit, a polyanion and a free (CH₃)₂NH molecule. The ESR spectrum of the title compound shows that charge-transfer between organic groups and polyanion takes place under irradiation of the sunlight in solid state. The TG study of the title compound shows that it had four stages of the weight loss, and the increase of the de-composition temperature for the polyanion shows that the stability of the polyanion was enhanced due to the influence of Zn²⁺ ion. CCDC:175866.     

Facile Heteropolyacid-Promoted Synthesis of Indeno[1,2-b]quinoline-9,11(6H,10H)-dione Derivatives

An efficient synthesis of indeno[1,2-b]quinoline-9,11(6H,10H)-dione derivatives was reported via four-component coupling reaction of aldehydes, dimedone, 1,3-indandione, and amines in refluxing ethanol or three-component condensation of aldehydes, 1,3-indandione, and 5,5-dimethyl-3-arylamino-cyclohex-2-enone derivatives at 120 °C under solvent-free conditions in the presence of a catalytic amount of Preyssler-type heteropolyacid, H₁₄[NaP₅W₃₀O₁₁₀], as a green and reusable catalyst.