克拉霉素的晶型及其转换

Crystal Form and Transformation of Clarithromycin

摘要: 克拉霉素与柠檬酸成盐,在乙醇-水、丙酮-水、异丙醇-水(1∶1)中调碱,或与酒石酸成盐,在乙醇-水、丙酮-水(1∶1)中调碱,在常压60℃下干燥,DSC分析证明该晶型为FormⅡ.该工艺避免了真空高温干燥的转晶条件,易于工业化生成.同时得到了克拉霉素的乙腈加成物单晶:P21晶型,a=1.064 4(2)nm,b=1.809 9(4)nm,c=1.162 8(2)nm,α=γ=90°,β=95.38(3)°,V=2.230 1(8)nm3,Z=2,Dc=1.175 g.cm-3,μ=0.087 mm-1,F

Abstract: Form Ⅱof clarithromycin can easily be obtained by the process where by a salt of clarithromycin with citric acid is neutralized in ethanol-water,acetone-water,and isopropanol-water(1∶1),or a salt with tartaric acid is neutralized in ethanol-water,acetone-water(1∶1),followed by drying at 60 ℃ and on normal pressure.The process obviates the condition of vacuum and higher temperature drying,as reported in the literatures.DSC analysis proved the crystal to be of the Form Ⅱ.Additionally,the single crystal structure of clarithromycin acetonitrile adduct was obtained in monoclinic system,P21 space group,a=1.064 4(2) nm,b=1.809 9(4) nm,c=1.162 8(2) nm,α=γ=90°,β=95.38(3)°,V=2.230 1(8) nm3,Z=2,Dc=1.175 g/cm3,μ=0.087 mm-1,F(000)=860,R1=0.034,wR2=0.062.