公开(公告)号：US5675030A

公开(公告)日：1997-10-07

申请号：US340552

申请日：1994-11-16

申请人： Lalitha Krishnan ,  Richard A. Leese ,  Raghavan Krishnan

发明人： Lalitha Krishnan ,  Richard A. Leese ,  Raghavan Krishnan

IPC分类号： C07C237/26 ,  A61K31/65

CPC分类号： C07C237/26 ,  C07C2103/46

摘要： The invention provides a method for selectively extracting a compound of formula I: ##STR1## wherein: R is hydrogen or --NR.sub.3 R.sub.4 ; and when R=--NR.sub.3 R.sub.4, R.sub.3 and R.sub.4 may be the same or different and are selected from hydrogen and straight or branched (C.sub.1 -C.sub.4)alkyl; R.sub.1 and R.sub.2 may be the same or different and are selected from straight or branched (C.sub.1 -C.sub.6)alkyl; from an aqueous mixture containing a compound of Formula I, its C-4 epimer and its oxidative degradation by-products by adding methylene at a concentration of 2-4 ml of methylene chloride per gram of compound of Formula I and at a pH between pH 6.5-8.0; and obtaining an extract containing methylene chloride, a compound of Formula I, and its C-4 epimer, said epimer being present in an amount of less than 3% of the amount of the compound of Formula I.

摘要翻译： 本发明提供了选择性提取式I化合物的方法：其中：R是氢或-NR 3 R 4; 当R = -NR 3 R 4时，R 3和R 4可以相同或不同，并且选自氢和直链或支链（C 1 -C 4）烷基; R 1和R 2可以相同或不同，并且选自直链或支链（C 1 -C 6）烷基; 从含有式I化合物，其C-4差向异构体及其氧化降解副产物的含水混合物中加入浓度为2-4ml二氯甲烷/克式I化合物的亚甲基，pH在pH 6.5-8.0; 并得到含有二氯甲烷的提取物，式I化合物及其C-4差向异构体，所述差向异构体的存在量小于式I化合物的量的3％。

公开(公告)号：US4958020A

公开(公告)日：1990-09-18

申请号：US350966

申请日：1989-05-12

申请人： Raghavan Krishnan ,  Jesse Gamble ,  David Blum ,  William V. Curran ,  Ving J. Lee ,  Ransom B. Conrow

发明人： Raghavan Krishnan ,  Jesse Gamble ,  David Blum ,  William V. Curran ,  Ving J. Lee ,  Ransom B. Conrow

IPC分类号： C07D499/87 ,  A61K31/43 ,  A61P31/04 ,  C07D499/00 ,  C07D499/86 ,  C07D499/897

CPC分类号： C07D499/00

摘要： A process for producing the compound [2S-(2.alpha.,3.beta.,5.alpha.)]-3-methyl-7-oxo-3-(1H-1,2,3-triazol-1-yl-methyl)-4-thia-1-azabicyclo[3 2 0]-heptane-2-carboxylic acid, (4-nitrophenyl)methyl ester, 4,4-dioxide, which comprises reacting a solution of azidopenamsulfone, 4-methoxyphenol and vinylpropionate with a solution of bis(trimethylsilyl)acetamide and 4-methoxyphenol is toluene at 80.degree.-100.degree. C. for 18-30 hours followed by filtering the resulting solution and cooling the filtrate to 0.degree.-10.degree. C.