Synthesis and crystal structure determination of 3-phenyl-2-(2- phenylhydrazino)-4H-1-benzothiopyran-4-one

Metz C.R.; Knight J.D.; Pastine S.J.; Pennington W.T.; Beam C.F.

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Synthesis and crystal structure determination of 3-phenyl-2-(2- phenylhydrazino)-4H-1-benzothiopyran-4-one

机译：3-苯基-2-（2-苯基肼基）-4H-1-苯并噻喃-4-酮的合成及晶体结构测定

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A new type of substituted benzothiopyranone, 3-phenyl-2-(2-phenylhydrazino) -4H-1-benzothiopyran-4- one, has been prepared by the condensation-acid cyclization of polylithiated phenylacetic acid phenylhydrazide with lithiated methyl thiosalicylate. Absorption spectra, especially 13C NMR, provided good indication of its structure, which was conclusively established with X-ray rystal structure analysis. In comparison to the few benzothiopyran X-ray reports documented, the benzothiopyranone ring of the molecule was found to be essentially planar, with the 3-phenyl ring nearly perpendicular to the benzothiopyranone fused-ring system. Crystals of C_(21)H _(16)N_2OS are orthorhombic, P2_12_12 _1, a = 10.140(4) ?, b = 10.432(4) ?, c = 16.228(7) ?, Z = 4, V = 1717(1) ? ~3, R1 = 0.0267 and wR _2 = 0.0725 for reflections with I>2σ(I). The molecular packing in the crystal is the result of N-H?O hydrogen bonding.

机译：一种新型的取代苯并噻吩并吡喃酮，3-苯基-2-（2-苯并肼基）-4H-1-苯并噻吩并-4-，是通过多锂化苯乙酸苯肼与锂化硫代水杨酸甲酯的缩合酸环化反应制备的。吸收光谱，尤其是13 C NMR，很好地说明了其结构，这是通过X射线晶体结构分析得出的结论。与记录的少数苯并噻喃X射线报告相比，发现该分子的苯并噻吩并吡喃酮环基本上是平面的，其3-苯基环几乎垂直于苯并噻吩并吡喃酮稠环系统。 C_（21）H_（16）N_2OS的晶体是正交晶体，P2_12_12_1，a = 10.140（4）α，b = 10.432（4）α，c = 16.228（7）α，Z = 4，V = 1717（ 1）？〜3，对于I>2σ（I）的反射，R1 = 0.0267和wR _2 = 0.0725。晶体中的分子堆积是N-H2O氢键的结果。

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《Journal of chemical crystallography》 |2010年第6期|共5页
作者
Metz C.R.; Knight J.D.; Pastine S.J.; Pennington W.T.; Beam C.F.;
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正文语种 eng
中图分类晶体学;
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Phenylhydrazino-benzothiopyranone synthesis; X-ray analysis;

机译：苯肼基-苯并硫代吡喃酮的合成;X射线分析;

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Synthesis and crystal structure determination of 3-phenyl-2-(2- phenylhydrazino)-4H-1-benzothiopyran-4-one

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