1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲的合成及手性晶体结构

对二甲氨基苯甲醛和苯基氨基硫脲缩合反应生成对二甲氨基苯甲醛缩氨基苯硫脲{1-4-(dimethylamino)ben- zylidene]-4-phenylthiosemicarbazide}, 并从溶液中析出手性晶体. 元素分析、红外光谱、紫外光谱、核磁谱、质谱和X射线衍射测定其组成和结构. 晶体属正交晶系, P2₁2₁2₁空间群, a＝0.77038(14) nm, b＝1.1428(2) nm, c＝1.6726(3) nm, V＝1.4726(5) nm³, Z＝4, D_c＝1.346 g/cm³, F(000)＝632, μ＝0.219 mm^－1, 可观测点精修最终偏离因子: R＝0.0407, wR＝0.1157. 化合物的晶体结构和固态圆二色谱表明化合物在结晶过程中发生单一对映体的手性堆积.

Synthesis and Chiral Crystal Structure of 1-[4-(Dimethylamino)- benzylidene]-4-phenylthiosemicarbazide

The reaction of 4-phenylthiosemicarbazide with p-dimethylaminobenzaldehyde produced 1-4-(dimethylamino)benzylidene]-4-phenylthiosemicarbazide which was characterized by elemental analy-sis, IR, UV, ¹H NMR and XRD. The crystal belongs to orthorhombic system with space group P2₁2₁2₁ and a＝0.77038(14) nm, b＝1.1428(2) nm, c＝1.6726 nm, V＝1.4726(5) nm³, Z＝4, D_c＝1.346 g/cm³, F(000)＝632, μ＝0.219 mm^－1, the final R＝0.0407 and wR＝0.1157 for 2807 observed reflections I＞2σ(I)]. The crystal structure and the solid-state circular dichroism spectrum showed that an enantiomer of the compound packs into the chiral crystal.