The title compound C 13 H 9ClN 2(M=228.67) was prepared,and its single crystal was obtained.The crystal belongs to orthorhombic system,space group Pbca with cell parameters:a=0.70567(8),b=0.9978(2),c= 3.2464(4)nm ,V=2...The title compound C 13 H 9ClN 2(M=228.67) was prepared,and its single crystal was obtained.The crystal belongs to orthorhombic system,space group Pbca with cell parameters:a=0.70567(8),b=0.9978(2),c= 3.2464(4)nm ,V=2.2858(6)nm 3,Z=8,Dc=1.329kg/dm 3,F(000)=944,μ=0.305mm -1 .2377 independent reflections were collected,in which 1214[I>2σ(I)] reflections that could be observed were used for the structural analysis.The final refinement converged to R=0.0421,wR=0.0999,(Δ/σ) max =0.001,S=0.833.The dicyclic ring of benzimidazole and chlorobenzene ring formed a propeller configuration in the compound.展开更多
目的研究抗生素氟氯西林钠的关键中间体3-(2′-氯-6′-氟苯基)-5-甲基-4-异噁唑甲酰氯的合成方法,使之适合工业化生产。方法以2-氯-6-氟苯甲醛为原料,经肟化、氯化、环合、水解、酰氯化等步骤制得目标化合物。结果合成产物的化学结构经I...目的研究抗生素氟氯西林钠的关键中间体3-(2′-氯-6′-氟苯基)-5-甲基-4-异噁唑甲酰氯的合成方法,使之适合工业化生产。方法以2-氯-6-氟苯甲醛为原料,经肟化、氯化、环合、水解、酰氯化等步骤制得目标化合物。结果合成产物的化学结构经IR,1H-NMR,13C-NMR and MS确证,总收率为60.2%。结论此方法收率高,成本低,适合工业化生产。展开更多
文摘The title compound C 13 H 9ClN 2(M=228.67) was prepared,and its single crystal was obtained.The crystal belongs to orthorhombic system,space group Pbca with cell parameters:a=0.70567(8),b=0.9978(2),c= 3.2464(4)nm ,V=2.2858(6)nm 3,Z=8,Dc=1.329kg/dm 3,F(000)=944,μ=0.305mm -1 .2377 independent reflections were collected,in which 1214[I>2σ(I)] reflections that could be observed were used for the structural analysis.The final refinement converged to R=0.0421,wR=0.0999,(Δ/σ) max =0.001,S=0.833.The dicyclic ring of benzimidazole and chlorobenzene ring formed a propeller configuration in the compound.
基金supported by the National Basic Research and Development Program of China(973 Program,2011CB710800)New Century Excellent Talents in University(NCET-11-0658)+2 种基金Natural Science Foundation of Jiangsu Province(BK2011150)the Program of Introducing Talents of Discipline to Universities(111-2-06)a Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions~~
文摘目的研究抗生素氟氯西林钠的关键中间体3-(2′-氯-6′-氟苯基)-5-甲基-4-异噁唑甲酰氯的合成方法,使之适合工业化生产。方法以2-氯-6-氟苯甲醛为原料,经肟化、氯化、环合、水解、酰氯化等步骤制得目标化合物。结果合成产物的化学结构经IR,1H-NMR,13C-NMR and MS确证,总收率为60.2%。结论此方法收率高,成本低,适合工业化生产。
