摘要
标题化合物C20H22FNO4由4 氟苯亚甲基氰乙酸乙酯和5,5 二甲基 1,3 环己二酮在三乙基苄基氯化铵(TE BA)存在下在水中加热反应而得,结构通过单晶X射线衍射法确定,其晶体属三斜晶系,空间群P-1,Mr=359 39,a=0.8266(1)nm,b=0.9773(1)nm,c=1.2375(2)nm,α=81 40(1)°,β=73 41(1)°,γ=82 15(1)°,V=0.9426(2)nm3,Z=2,Dc=1.266g·mm-3,μ=0 094mm-1,F(000)=380,最终的偏离因子为R=0 0403,Rw=0 1057,在分子结构中平面1(苯环)与平面2(C(8)、C(13)、C(14)、C(15))之间的二面角为89 56°,平面2与平面3(C(8)、C(9)、C(10)、C(12)、C(13))之间的二面角为13 37°,平面1与平面3之间的二面角为102 70°.吡喃环为船式构象,而与吡喃环稠合的六元环为信封式构象.
The title compound (C20H22FNO4) has been synthesized by the reaction of ethyl 4fluorobenzylidenecyanoacetate with 5,5dimethyl1,3cyclohexaneclione in water in the presence of triethylbenzylammonium chloride (TEBA),and its structure was determined by monocrystalline Xray diffraction. The crystal is triclinic, space group P-1 with a=0.826 6(1) nm, b=0.977 3(1) nm, c=1.237 5(2) nm, α=8140(1)°, β=7341(1)°, γ=8215(1)°,Z=2,V=0.942 6(2) nm3,Mr=35939,Dc=1266 g·mm-1,μ (Mo Kα)=0094 mm-1, F(000)=380, The structure was solved by direct methods and refined by the fullmatrix method of leastsquares to the final R=0040 3 and Rw=0105 7. Xray analysis reveals that the dihedral angle between plane 1 (phenyl ring) and plane 2 (C(8), C(13), C(14), C(15)) is 8956°, between plane 2 and plane 3 (C(8), C(9), C(10), C(12), C(13)) is 1337°,between plane 1 and plane 3 is 10270°,the pyran cycle and the sixmembered cycle fused with it are of boat and envelope configurations in the structure respectively.
出处
《徐州师范大学学报（自然科学版）》
CAS
2003年第2期46-49,共4页
Journal of Xuzhou Normal University(Natural Science Edition)
