The invention discloses a method for preparing high-purity torasemide and a crystal form I thereof. The method comprises the following steps of: reacting 4-chloro-3-pyridine sulfonamide and m-toluidine serving as raw materials to obtain 3-sulfamoyl-4-(3-methyl phenyl) aminopyridine, refining, and reacting with 1,1'-carbonyldimidazole and isopropamide, directly introducing isopropyl carbamyl, thus obtaining the high-purity torasemide, wherein the purity (high performance liquid chromatography (HPLC)) of the torasemide is more than 99.5 percent. The prepared torasemide has proper granularity, seed crystal is not required for crystal transformation, the torasemide can be directly transformed into the variant crystal form I, and a chemically pure torasemide variant I is obtained. The preparation method is strong in process controllability, easy and convenient to operate and high in reproducibility, and facilitates industrialized production.

Objective To synthesize three specified impurities as reference substances for strengthening quality control of fludarabine phosphate.Methods 6-Amino-9-(5-O-phosphono-β-D-arabinofuranosyl)-9H-purin-2-ol(impurity A)and 2-ethoxy-9-(5-O-phosphono-β-D-arabinofuranosyl)-9H-purin-6-amine(impurity F)were synthesized from 9-(5-O-phosphono-β-D-arabinofuranosyl)-2-fluoro-9H-purin-6-amine(fludarabine phosphate)through substitution reaction,and 9-(3,5-di-O-phosphono-β-D-arabinofuranosyl)-2-fluoro-9H-purin-6-amine(impurity C)was synthesized from 9-β-D-arabinofuranosyl-2-fluoro-9H-purin-6-amine(impurity E)through phosphorylation and hydrolysis.Reversed-phase HPLC was used to purify the impurities.Results Three specified impurities of fludarabine phosphate were obtained,and their structures were identified by HR-MS and NMR.Conclusions The obtained compounds can be used as reference substances for the qualitative and quantitative analysis of fludarabine phosphate related substances.

在互联网的搜索栏,只需输入"豪赌镇长张健"字样,即可出现相关消息近4万条。近日记者前往江苏省海门市德胜镇采访时,当地群众颇有些无奈地称:"这下德胜镇可出名了。"给德胜镇带来如此之大"名声"的,正是原镇长张健。张健在任职期间,以招商引资、建设农民集中居住示范区项目为名,贪污、诈骗1445万元,40余次出境赌博血本无归,最终走上了一条不归路。2006年12月14日,江苏省南通市中级人民法院一审以贪污罪、诈骗罪、受贿罪判处张健无期徒刑,剥夺政治权利终身,并处没收个人全部财产。

从原料、配方、设备、工艺方面提出生产优质PVC-U异型材模塑料的方法,及模塑料的质量检测方法.

通过将几种多取代芳烃按适当比例复配,加入螯合剂等稳定成分以抑制残余催化剂在高温下对产品和溶剂的分解,组成复合溶剂,用以重结晶纯化十溴二苯醚粗品.该溶剂对十溴二苯醚具有理想的溶解度-温度梯度,能彻底去除粗品中的游离溴,所得产品纯度高,热稳定性好,不含游离溴.本工艺操作简便,溶剂易于回收,精制费用低廉.

以石油醚为溶剂，无水氯化锌为催化剂，用三氯化磷和水反应发生氯化氢气体，同联苯、多聚甲醛进行氯甲基化反应，合成４，４＇－二（氯甲基）联苯，收率达到６４％，产品熔点１３２￣１３５℃，提出了最佳工艺条件。