SYNTHESIS AND CRYSTAL STRUCTURE OF La（NO3）3（16—C—5）

<正> The title complex LaC11H22O14N3 (Mr = 559. 27) crystallizes in the monoclinic space group P21/c with a=14. 452(7) ,b=8. 260(2),c= 16. 641(8) A ,β= 90. 85(4)°, Z = 4, V=1986. 2(1) A3,Dc=1. 87g·cm-3, F(000) = 1112,μ(MoKa) = 22. 7cm-1. The final refinement converged with R=0. 036 and Rw = 0. 038 for 2996 observed independent reflectios. The average La-O(crown) bond length of 2. 683 A (2. 660-2. 701A)is shorter than that in La(NO3)3(15-C-5)(2. 694A).The distances between opposite O atoms (3. 47~4. 68A) indicate that the cavity of 16-C-5 in the complex is elliptic.     

1，3—Dipolar Cycloaddition of Substituted Benzonitrile Oxide to 5—（R）—（1—Menthyloxy）—2（5H）—furanone

Several isoxazoline compounds were obtained by the 1,3-dipolar cycloaddition of benzonitrile oxide to 5-(R)-(1-menthyloxy)-2(5H)-furanone. The reaction condition was investigated preliminarily, the structures of these compounds have been established via the analysis of NMR data (involved NOEID or HMBC) and the reaction seems occurred regioselectively.     

CRYSTAL STRUCTURE OF（η^5—C5H5）GdCl2（THF）3

<正> Compound (η5-C5H5)GdCl2(THF)3 was successfully prepared from action of GdCl3 and NaC5H5 in tetrahydrofuran (THF). X-ray diffraction data were collected at low temperature (about 210K). Its crystal belongs to the monoclinic space group P 21/n with a = 7. 821(2), b = 17.068(1), c=15. 057(1)(?), β=94. 76 (2)°, V = 2003. 2(10)(?)3, Z = 4, Dc=1. 69g/cm3, F(000)=1012, Mr=509. 6. The structure was solved by heavy-atom method. Least-squares refinement converged to a final R value of 0. 050. The coordination number of the Gd atom is 8. The centre of the cyclopentadienyl, the two Cl atoms and the three oxygen atoms of THF molecules form a distorted octahedron about the Gd atom.     

Crystal Structure of 5—（l—Menthyloxy）—3—chloro—4— Pyrrolidinyl—2（5H0—f

The molecular structure of the title compound 5-(l-menthyloxy)-3-chloro-4-pyrrolidinyl-2(5H)-furanone, C18H28ClNO3(Ⅰ), has been determined by X-ray diffraction at 296(1)K. The crystal is monoclinic with space group P21, a=9.457(3), b=10.413(3), c=9.525(2), β=95.19(2)°, V=934(1) 3, Z=2, Mr=341.88, Dx=1.22 g/cm3, μ=2.15 cm-1, F(000)=368. The final R factor is 0.059, and Rw is 0.065 for 1020 observed reflections with I≥3σ(I). The absolute configuration at C(14) of the acetal carbon was proved to be S, taking into account the known configuration of 1R, 2S, 5R-menthyl moiety. There are three rings in the molecule of this compound: the furanone ring, the pyrrolidine ring and the mentholoxy group ring. The franone ring is connected with the pyrrolidine ring and the mentholoxy ring by N atom and μ2-O bridge atom respectively.     

（3—苄基—4—芳酰基—1,2,4—三唑—5—基）（5—苯基—1,3,4—E…

通过３－苄基－４－芳酰基－１，２，４－三唑－５－巯基负离子在２－甲磺酰基－５－苯基－１，３，４－Ｅ二唑环２－位上的亲核取代反应，制得１３个新的（３－苄基－４－芳酰基－１，２，４－三唑－５－基）（５－苯基－１，３，４－Ｅ二唑－２－基）硫醚衍生物。经元素分析、ＩＲ、＾１Ｈ ＮＭＲ和ＭＳ裂解碎片分析确认结构。初步观察了它们在０．０１％浓度时对大肠杆菌繁殖的抑制作用。     

3—（3‘—羟基丁基）异苯并呋喃—1（3H）—酮的合成

由邻苯二甲酸酐为原料，经中间体３－羟基苯酞（３），再经溴丙烯及锡存在下３的烯丙基化、硼氢化氧化、铬酐氧化，二甲基锌甲基化，共６步反应合成了３－（３‘－羟基丁基）异苯并呋喃－１（３Ｈ）－酮。