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  

作　　者：孙海燕 佘能芳 

机构地区：[1]NanJing Polytechnic institute [2]Key Laboratory of Pesticide and Chemical Biology of Ministry of Education of China, College of Chemistry, Central China Normal University

出　　处：《Chinese Journal of Structural Chemistry》2016年第7期1054-1058,共5页结构化学（英文）

基　　金：Project supported by the National Natural Science Foundation of China(No.21272086)

摘　　要：A new compound [C19H19N3O3F2Cl·C4H3O4·H2O]（I）,（7-（（7S）-7-aminospiro[2.4]heptan-5-yl）-8-chloro-6-fluoro-1-（（1R,2S）-2-fluorocyclopropyl）-4-oxo-1,4-dihydroquinoline-3-carboxylic acid fumaric acid monohydrate）, was synthesized and structurally characterized by single-crystal X-ray diffraction, ^1H NMR, 14 C 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） A, β = 103.37（1）°, V = 1226.8（5） A^3, Z = 2, Mr = 543.90, Dc = 1.472 g/cm^3, 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]heptan-5-yl）-8-chloro-6-fluoro-1-（（1R,2S）-2-fluorocyclopropyl）-4-oxo-1,4-dihydroquinoline-3-carboxylic acid fumaric acid monohydrate）, was synthesized and structurally characterized by single-crystal X-ray diffraction, ^1H NMR, 14 C 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） A, β = 103.37（1）°, V = 1226.8（5） A^3, Z = 2, Mr = 543.90, Dc = 1.472 g/cm^3, 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.

关 键 词：sitafloxacin synthesis crystal structure 

分 类 号：TQ460.1[化学工程—制药化工]