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| Synthesis and Crystal Structure of Diethyl-2,6- dimethyl-3,5- diyl- （ 1- （2- chlorob enzoyl）- 1H- pyrazole-3-diethyl-carboxylate）-pyridine | |
| 引用本文： | QIAN Quna ZHANG Mina②LI Zhi-Fena CAO Wei-Guoa ZHANG Juna SHAO Minb XIA Yi-Benca. Synthesis and Crystal Structure of Diethyl-2,6- dimethyl-3,5- diyl- （ 1- （2- chlorob enzoyl）- 1H- pyrazole-3-diethyl-carboxylate）-pyridine[J]. 结构化学, 2008, 27(10): 1163-1166 |
| 作者姓名： | QIAN Quna ZHANG Mina②LI Zhi-Fena CAO Wei-Guoa ZHANG Juna SHAO Minb XIA Yi-Benca |
| 作者单位： | Department of Chemistry，Shanghai University，Instrumental Analysis and Research Center，Shanghai University，School of Materials Science and Engineering，Shanghai University |
| 基金项目： | 上海市教育厅重点项目，Foundation of Education Commission of Shanghai Municipality |
| 摘 要： | The reaction of hydrazine hydrate with a new α,γ-diketone ester 3, derived from the reaction of 2,6-dimethyl-3,5-diacetyl-pyridine 2 with diethyl oxalate in the presence of sodium ethoxide, afforded the pyrazole derivative 4. Treatment of 4 with 2-chlorobenzoyl chloride gave diethyl 2,6-dimethyl-3,5-diyl-（1-2（chlorobenzoyl）-1H-pyrazole-3-diethyl-carboxylate） pyridine 5. Fine crystal of 5 suitable for XRD analysis was obtained form recrystalization in ethyl acetate. The crystal belongs to the triclinic system, space group P1^-, with a = 1.0342（11）, b = 1.2211（12）, c = 1.5013（15） nm, α = 82.5190（10）,β = 85.7960（10）,γ = 85.3150（10）°, V= 1.8697（3） nm^3, Dc= 1.173 g/cm^3, μ = 0.219 mm^-1, F（000） = 684, Z = 2, the final R = 0.0720 and wR = 0.2211. |
| 关 键 词： | 吡啶 N-酰化 晶体结构 化学分析 |
Synthesis and Crystal Structure of Diethyl-2,6-dimethyl-3,5-diyl-(1-(2-chlorobenzoyl)-1H-pyrazole-3-diethyl-carboxylate)-pyridine |
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| QIAN Qun,ZHANG Min,LI Zhi-Fen,CAO Wei-Guo,ZHANG Jun,SHAO Min,XIA Yi-Ben. Synthesis and Crystal Structure of Diethyl-2,6-dimethyl-3,5-diyl-(1-(2-chlorobenzoyl)-1H-pyrazole-3-diethyl-carboxylate)-pyridine[J]. Chinese Journal of Structural Chemistry, 2008, 27(10): 1163-1166 | |
| Authors: | QIAN Qun ZHANG Min LI Zhi-Fen CAO Wei-Guo ZHANG Jun SHAO Min XIA Yi-Ben |
| Affiliation: | 1. Department of Chemistry, Shanghai University, Shanghai 200444, China 2. Instrumental Analysis and Research Center, Shanghai University, Shanghai 200444, China 3. School of Materials Science and Engineering, Shanghai University, Shanghai 200444, China |
| Abstract: | The reaction of hydrazine hydrate with a new α,γ-diketone ester 3, derived from the reaction of 2,6-dimethyl-3,5-diacetyl-pyridine 2 with diethyl oxalate in the presence of sodium ethoxide, afforded the pyrazole derivative 4. Treatment of 4 with 2-chlorobenzoyl chloride gave diethyl 2,6-dimethyl-3,5-diyl-(1-2(chlorobenzoyl)-1H-pyrazole-3-diethyl-carboxylate) pyridine 5. Fine crystal of 5 suitable for XRD analysis was obtained form recrystalization in ethyl acetate. The crystal belongs to the triclinic system, space group P, with a = 1.0342(11), b = 1.2211(12), c = 1.5013(15) nm, α = 82.5190(10), β = 85.7960(10), γ = 85.3150(10)°, V = 1.8697(3) nm3, Dc = 1.173 g/cm3, μ = 0.219 mm-1, F(000) = 684, Z = 2, the final R = 0.0720 and wR = 0.2211. |
| Keywords: | pyridine pyrazole N-acylation crystal structure |
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