Synthesis and Crystal Structure of 7-((7S)-7-Aminospiro[2.4]heptan-5-yl)-8-chloro- 6-fluoro-1-((1R,2S)-cis-2-fluorocyclopropyl)-4-oxo-1,4-dihydroqun-oline-3-carboxylic Acid Fumaric Acid Monohydra
孙海燕;佘能芳
a (NanJing Polytechnic institute, Nanjing 210048, China)
b (Key Laboratory of Pesticide and Chemical Biology of Ministry of Education of China, College of Chemistry, Central China Normal University, Wuhan 430079, China)
Synthesis and Crystal Structure of 7-((7S)-7-Aminospiro[2.4]heptan-5-yl)-8-chloro- 6-fluoro-1-((1R,2S)-cis-2-fluorocyclopropyl)-4-oxo-1,4-dihydroqun-oline-3-carboxylic Acid Fumaric Acid Monohydra
SUN Hai-Yan;SHE Neng-Fang
a (NanJing Polytechnic institute, Nanjing 210048, China)
b (Key Laboratory of Pesticide and Chemical Biology of Ministry of Education of China, College of Chemistry, Central China Normal University, Wuhan 430079, China)
A new compound [C19H19N3O3F2Cl∙C4H3O4∙H2O] (I), (7-((7S)-7-aminospiro[2.4]hep- tan-5-yl)-8-chloro-6-fluoro-1-((1R,2S)-2-fluorocyclopropyl)-4-oxo-1,4-dihydroquinoline-3-carb-oxylic acid fumaric acid monohydrate), was synthesized and structurally characterized by single-crystal X-ray diffraction, 1H NMR, 14C spectra and mass spectra. I crystallizes in monoclinic, space group P21/c with a = 8.495(2), b = 12.545(3), c = 11.832(3) Å, β = 103.37(1)°, V = 1226.8(5) Å3, Z = 2, Mr = 543.90, Dc = 1.472 g/cm3, F(000) = 564, μ = 0.225 mm-1, the final R = 0.0307 and wR = 0.0892 for 6886 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the quinolinone ring is almost coplanar, and the pyrrole ring adopts an envelope form. Packing of crystal I is constructed and stabilized by the N–H•••O, O–H•••O and N–H•••Cl hydrogen bonds together with C–H•••π interations.
A new compound [C19H19N3O3F2Cl∙C4H3O4∙H2O] (I), (7-((7S)-7-aminospiro[2.4]hep- tan-5-yl)-8-chloro-6-fluoro-1-((1R,2S)-2-fluorocyclopropyl)-4-oxo-1,4-dihydroquinoline-3-carb-oxylic acid fumaric acid monohydrate), was synthesized and structurally characterized by single-crystal X-ray diffraction, 1H NMR, 14C spectra and mass spectra. I crystallizes in monoclinic, space group P21/c with a = 8.495(2), b = 12.545(3), c = 11.832(3) Å, β = 103.37(1)°, V = 1226.8(5) Å3, Z = 2, Mr = 543.90, Dc = 1.472 g/cm3, F(000) = 564, μ = 0.225 mm-1, the final R = 0.0307 and wR = 0.0892 for 6886 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the quinolinone ring is almost coplanar, and the pyrrole ring adopts an envelope form. Packing of crystal I is constructed and stabilized by the N–H•••O, O–H•••O and N–H•••Cl hydrogen bonds together with C–H•••π interations.
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2016, Vol. 35 
