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目的研发一种新型唑烷酮类抗生素((3R,3a S)-7-(6-((S)3-甲基-2-唑烷酮-5-基)吡啶-3-基)-1-氧-1,3,3a,4-四氢苯并[b]唑[3,4-d][1,4]嗪-3-基)甲基)磷酸单酯(TJ1508)的合成工艺,并研究其晶型。方法以磷酸二苄酯中间体为原料,通过酸催化脱苄基得到TJ1508,在不同的溶剂体系中析晶得到不同晶型,采用粉末X射线衍射分析(PXRD)和差示扫描量热分析(DSC)对其进行表征,并对其进行加速稳定性试验和溶剂残留检测。结果目标化合物的收率最高为89%,得到3种不同的晶型A、B和C,稳定性、溶剂残留和钯残留均优于化合物专利无定型产品。结论设计了一种TJ1508的简易合成路线,得到3种稳定的晶型,其中晶型C最为稳定。
Objective To develop a novel oxazolidinone antibiotic ((3R, 3aS) -7- (6 - ((S) 3-methyl-2-oxazolidinon-5-yl) (TJ1508) was synthesized by the same method as described in example 1, except that the above-mentioned compound And study its crystal form. Methods TJ1508 was obtained by the debenzylation of acid with dibenzyl phosphate as intermediate. Different crystal forms were obtained by crystallization from different solvent systems. The results of powder X-ray diffraction (XRD) and differential scanning calorimetry DSC), and its accelerated stability test and solvent residue detection. As a result, the yield of the target compound was 89% at the highest, three different crystal forms A, B and C were obtained, and the stability, solvent residue and palladium residue were superior to the compound patent amorphous product. Conclusion A simple synthesis of TJ1508 was designed and three stable crystalline forms were obtained, of which Form C was the most stable.