(E)-4-(3-(二甲氨基)丙-1-烯基)苯酚新晶体的合成及结构研究

Synthesis and crystal structure of (E)- 4-(3-(dimethylamino)prop-1- enyl) phenol

以甲醛、二甲胺和对羟基肉桂酸为原料,采用一锅煮的合成方法得到(E)-4-(3-(二甲氨基)丙-1-烯基)苯酚(EDP)产物粗产品,再根据产物与原料的不同物化性质,采用简单而且省时省力的沉淀法和重结晶法分离纯化得到一种无色块状晶体化合物,质谱和X-射线单晶衍射结果显示,该晶体为单斜晶系,空间群为P2(1)/c,晶体的其他相关参数:a=18.060(14),b=9.742(8),c=12.710(10),α=90°,β=109.829(9)°,γ=90°,V=2 104(3)3,Z=8,F(000)=768.0,晶体密度Dc=1.119 mg/m3,化合物分子量Mr=177.24,衍射波长λ=0.710 73,可观察衍射点R=0.047 5,全部衍射点wR=0.145 0,独立衍射点中强度大于2σ的衍射点数为3 542。通过查新,获知该物质为新的化合物。

（E）-4-（3-（dimethylamino）prop-1-enyl）phenol（EDP） was synthesized by the reaction of （ E ）-3-（ 4-hydroxyphenyl ） acrylic acid with dimethylamine and formaldehyde through one-pot method and purified by the simple precipitation and recrystallization based on the difference of the physical and chemical properties between the product and raw materials.EDP was characterized by ESI -MS and X-ray single-crystal diffraction.Its crystal is monoclinic, space group P2 （ 1 ）/c with a=18.060 （ 14 ） ？, b=9.742 （ 8 ） ？, c=12.710 （ 10 ） ？, α=90 °, β=109.829 （ 9 ） °, γ=90 °, V=2 104（3）？3 , Z=8, F（000）=768.0, Dc=1.119 mg/m^3 , Mr=177.24,λ=0.710 73 ？, the final R=0.047 5 and wR=0.145 0 for 3 542 observed reflections with I 〉2σ（ I ）.Through the checking for new, EDP is proved to be a new compound.