A series of novel calix[4]arene derivatives incorporating two triazolyl 1 3-diketo subunits in alternate positions at the lower rim were synthesized and screened for HⅣ integrase inhibition activity.The chemical structures of these compounds were confirmed by means of1H NMR 13C NMR,and ESI-MS.Preliminary bioassays indicated that calix[4]arene derivatives proved to be more active than p-tertbutylcalix[4]arene derivatives.In particular,compound 4g presented the most potent integrase strand transfer inhibitory activity with an IC50value of 6.1 mmol/L.
Zai-Gang LuoYu ZhaoChao MaXue-Mei XuXiao-Mei ZhangNian-Yu HuangHong-Qiu He
Two 1-methyl-1H-benzo[d]imidazole derivatives, C_（18）H_（14）CuN_4O_4·C_4H_8O_2（1） and C_9H_9N_3O（2）, have been synthesized and characterized by NMR, MS, FT-IR, elementary analysis and X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group P2_1/n with a = 9.6888（3）, b = 7.3772（2）, c = 14.3277（4）A, β = 95.819（3）°, V = 1018.81（5） A3, M_r = 501.98, Z = 2, D_c = 1.636 g/cm^3, F（000） = 518, μ = 1.123 mm^（-1）, MoKα radiation（λ = 0.71073 A）, the final R = 0.0325 and wR = 0.0859 for 1821 observed reflections with I 〉 2σ（I）. Compound 2 crystallizes in monoclinic, space group C2/c with a = 14.2908（14）, b = 14.4268（13）, c = 8.4802（6） A, β = 108.513（9）o, V = 1657.9（3） A3, M_r = 175.19, Z = 8, D_c = 1.404 g/cm^3, F（000） = 736, μ = 0.097 mm^（-1）, Mo Kα radiation（λ = 0.71073 A）, the final R = 0.0563 and wR = 0.1531 for 1231 observed reflections with I 〉 2σ（I）. Intermolecular（N-H···N, N-H···O） and intramolecular（N-H···N, C-H···O） hydrogen bonds, as well as C-H···π and π-π stacking interactions, help to stabilize the crystal structure of compound 2.
Two new thieno[2,3-d]pyrimidin-4（3H）-one derivatives,C24H22 Cl N3O2S（5a） and C25H25N3O2S（5b）,have been synthesized via a tandem aza-Wittig reaction.This tandem reaction has many attractive aspects such as easily accessible and versatile starting materials,mild conditions and high yields.Both compounds have been characterized by elemental analysis,HR-MS,IR,NMR spectra and X-ray single-crystal diffraction.Compound 5a crystallizes in monoclinic,space group P21/c with a = 9.986（3）,b = 14.263（4）,c = 15.530（5）A,β = 93.806（5）o,V = 2207.1（11） A^3,Mr = 451.96,Z = 4,Dc = 1.360 g/cm3,F（000） = 944,μ = 0.294 mm-1,Mo Kα radiation（λ = 0.71073 A）,the final R = 0.0444 and w R = 0.1219 for 3407 observed reflections with I 〉 2σ（I）.Compound 5bcrystallizes in triclinic,space group P1 with a = 8.974（4）,b = 10.766（5）,c = 12.260（6） A,β = 93.047（7）o,V = 1122.1（9） A^3,Mr = 431.54,Z = 2,Dc = 1.277 g/cm3,F（000） = 456,μ = 0.170 mm-1,Mo Kα radiation（λ = 0.71073 A）,the final R = 0.0378 and w R = 0.1072 for 3806 observed reflections with I 〉 2σ（I）.The preliminary antibacterial activities of 5a and 5b were investigated.Compound 5a showed 71.3% and 79.2% in vitro inhibition against Fusarium oxysporium and Rhizoctonia solani,respectively.Compound 5b showed 75.3% in vitro inhibition against Rhizoctonia solani.
LI Rong-KunYANG Quan-LiHUANG Nian-YuCHEN HongLIU Ming-Guo
Compound 1 （5-hydroxy-6-methoxybenzofuran-3-yl）（4-methoxyphenyl）metha- none, C17H1405, as a potential anti-breast cancer agent has been synthesized under microwave irradiation, which was further converted to （5,6-dihydroxybenzofuran-3-yl）（4-methoxyphenyi）me- thanone （2）. The compounds were characterized by MS and NMR spectra. Meanwhile, the crystal of 1 was obtained and determined by X-ray single-crystal diffraction. Crystal data： monoclinic system, space group P2/n, a = 8.908（6）, b = 10.505（7）, c = 15.452（11） A, β = 105.043（9）, V = 1396.4（16） A3, Z = 4, F（000） = 624, Dc = 1.419 g/cm3, p = 0.105 mm-1, R = 0.0513 and wR = 0.1246 for 14459 independent reflections （Rint = 0.0647） and 2488 observed ones （I〉 2σ（/））. lntermolecular O-H...O and π-π stacking interactions contributed to the stability of the structure.
The crystal structure of the new title compound （E）-ethyl 6-benzyl-2-[（cyclopropylmethylamino）（4-fluorophenylamino）methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate （C28H31FN 4O2S·C2H6O, Mr=552.70） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a=13.806（10）, b=10.850（7）, c=19.938（14）, β=98.842（9）° , V=2951（4）3 , Z=4, Dc=1.244g/cm 3 , F（000）=1176, μ=0.153 mm-1 , MoKα radiation （λ=0.71073）, R=0.0758 and wR=0.2234 for 4262 observed reflections with I 〉 2σ（I）. Intramolecular N-H…S and C-H…N interactions as well as intermolecular N-H…O and O-H…N hydrogen bonds help to stabilize the crystal structure. X-ray diffraction analysis reveals that the asymmetric unit contains one title molecule and one ethanol molecule.
Compound（Z）-2-methyl-5,6-dihydrobenzo[d]thiazol-7（4H）-one O-prop-2-yn-1-yl oxime, C11H12N2 OS, as a synthetic precursor of cytotoxic triazoles has been prepared and characterized by NMR spectra. Meanwhile, the crystal of IV was obtained and determined by X-ray single-crystal diffraction. Crystal data： monoclinic system, space group P21/c, a = 9.725（9）, b = 8.068（7）, c = 14.452（13）A, β = 98.68（2）°, V = 1120.9（17）A3, Z = 4, F（000） = 464, Dc = 1.305 g/cm^3, μ = 0.263 mm^-1, R = 0.0457 and w R = 0.1298 for 11511 independent reflections（Rint = 0.0709） and 2289 observed ones（I 〉 2σ（I））.
