| Synthesis of （3aS,6aR）- 1,3-Dibenzyl-tetrahydro- 1H-thieno[3,4-d]-imidazole-2（3H）-one-4-ylidenepentanoic Acid and Characterization of Its Crystal |
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| 引用本文： | 袁建莉,王静梅,陈芬儿.Synthesis of （3aS,6aR）- 1,3-Dibenzyl-tetrahydro- 1H-thieno[3,4-d]-imidazole-2（3H）-one-4-ylidenepentanoic Acid and Characterization of Its Crystal[J].结构化学,2004,23(6):507-510. |
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| 作者姓名： | 袁建莉 王静梅 陈芬儿 |
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| 作者单位： | YUAN Jian-Li a WANG Jing-Mei b CHEN Fen-Er a② a (Department of Chemistry，Fudan University，Shanghai 200433，China) b (Research Center for Analysis and Measurement，Fudan University，Shanghai 200433，China) |
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| 基金项目： | a Grant-in-Aid (96107) for Scientific Research from the Ministry of Chemical Industry of China |
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| 摘 要： | 1 INTRODUCTION The title compound, (3aS,6aR)-1.3-dibenzyl- tetrahydro-1H-thieno3,4-d]-imidazole-2(3H)-one- 4-ylidenepentanoic acid 3, is a key intermediate for the synthesis of d-biotin 1 (VITH, Fig. 1) which has been widely used not only as a pharmaceu…
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| 关 键 词： | 合成 晶体结构 维生素D 中间体 （3aS 6aR）-1 3-联苄基-四氢-4H-噻吩并[3 4-d]-咪唑-2，4（1H）-二酮 格林尼亚反应 |
Synthesis of (3aS,6aR)-1,3-Dibenzyl-tetrahydro- 1H-thieno[3,4-d]-imidazole-2(3H)-one-4-ylidenepentanoic Acid and Characterization of Its Crystal |
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| YUAN Jian-Li,WANG Jing-mei,CHEN Fen-Er.Synthesis of (3aS,6aR)-1,3-Dibenzyl-tetrahydro- 1H-thieno[3,4-d]-imidazole-2(3H)-one-4-ylidenepentanoic Acid and Characterization of Its Crystal[J].Chinese Journal of Structural Chemistry,2004,23(6):507-510. |
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| Authors: | YUAN Jian-Li WANG Jing-mei CHEN Fen-Er |
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| Institution: | Department of Chemistry, Fudan University, Shanghai 200433, China;Research Center for Analysis and Measurement,Fudan University, Shanghai 200433, China |
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| Abstract: | The intermediate of d-biotin, (3aS,6aR)-1,3-dibenzyltetrahydro-1H-thieno3,4- d]-imidazole-2(3H)-one-4-ylidenepentanoil acid was synthesized from (3aS,6aR)-1,3-dibenzylte- trahyro-4H-thieno3,4-d]-imidazole-2,4(1H)-dione by using the Grignard reaction. The structure of 3 was characterized by IR, 1H NMR and MS, and the absolute configuration was further confirmed by X-ray crystal structure analysis. Compound 3 crystallizes in monoclinic, space group P21 with a = 11.030(2), b = 7.783(2), c = 12.797(2) , b = 93.44(1)o, Z = 2, Mr = 422.53 (C24H26N2O3S), V = 1096.3(6) 3, = 0.177 mm-1, Dc = 1.280 g/cm3, F(000) = 448 and T = 293(2) K. The final R = 0.0737 and Rw = 0.1974 for 1009 observed reflections with I >2s(I). |
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| Keywords: | Grignard reaction synthesis X-ray crystal structure |
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