4,4'-一氧二(苯胺灵)的合成和晶体结构

Synthesis and Crystal Structure of 4,4′ Oxobis(propham)

通过4,4'-一氧二(异氰酸苯酯)与异丙醇加成反应,合成标题化合物4,4'-一氧二(苯胺灵)(Ⅰ)(C20H24N2O5,Mr=372.41),并用X射线衍射、红外光谱、13C核磁共振、电子轰击质谱和元素分析对标题化合物进行表征.晶体属于三斜晶系,空间群为P1.晶体学参数为:a=0.85107(17),b=0.91164(18),c=1.45701(3)nm,α=80.44(3)°,β=85.25(3)°,γ=62.88(3)°,V=0.9922(3)nm3,Z=2,Dc=1.247g·cm-3,μ(MoKα)=0.90cm-1,F(000)=396.两个苯环平面之间的夹角为62.06°(0.06°).晶体结构经全矩阵最小二乘法修正,最终偏离因子R=0.0520,wR=0.1434(对可观察点).此化合物应具有广谱的生物活性.

The title compounds 4, 4'-oxobis (propham) (I) (C20H24N2O5, M-r = 372.41) was synthesized by the addition reaction of the corresponding 4, 4'-oxobisphenyl diisocyanate with isopropanol. The crystal structure was determined by X-ray diffraction method. The crystal is of triclinic system, space group PI with a = 0.85107 (17), b = 0.91164 (18), c = 1.45701 (3) nm, alpha = 80.44 (3)degrees, beta = 85.25 (3)degrees , gamma = 62.88 (3)degrees, V = 0.9922 (3) nm(3), Z = 2, D-c = 1.247 g (.) cm(-3), mu(MoKalpha) = 0.90 cm(-1), F(000) = 396, R = 0.0520, wR = 0.1434 for 4336 observed reflections with [ I > 2sigma (I)]. X-ray analysis reveals that interatomic distances for O(2) - C (7) is 0.12142 (19), O(4) - C(17) is 0.12136 (18) nm, this obviously shows the formation of C = O double bonds and distances N1...O4 = 0.295310 nm and N2...O2 = 0.2941 nm show the formation of a weak hydrogen bonds.