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有机化学
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有机化学 ›› 2006, Vol. 26 ›› Issue (07): 933-936. 上一篇    下一篇

研究论文

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

俞芸1,2，林丽榕2，杨开冰2，章慧2，黄荣彬*,2，郑兰荪2,3   

  1. (1龙岩学院化学与材料工程系 龙岩 364000)
    (2厦门大学化学系 厦门 361005)
    (3固体表面物理化学国家重点实验室 厦门 361005)
  • 收稿日期:2005-07-15 修回日期:2006-01-11 发布日期:2006-07-01
  • 通讯作者: 黄荣彬

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

YU Yun1,2,LIN Li-Rong2,YANG Kai-Bin2,ZHANG Hui2
HUANG Rong-Bin*,2,ZHENG Lan-Sun2,3   

  1. (1 Department of Chemistry and Materials Engineering, Longyan College, Longyan 364000)
    (2 Department of Chemistry, Xiamen University, Xiamen 361005)
    (3 State Key Laboratory for Physical Chemistry of Solid Surface, Xiamen 361005)
  • Received:2005-07-15 Revised:2006-01-11 Published:2006-07-01
  • Contact: HUANG Rong-Bin*

PDF

1243

被引次数

41

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, Dc＝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.

关键词: 1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲, 合成, 圆二色谱, 手性晶体结构

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, Dc＝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.

Key words: synthesis, chiral crystal structure, circular dichroism spectrum, 1-[4-(dimethylamino)benzylidene]-4-phenylthiosemicarbazide