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1. 发明专利

JPH05294990A 失效
公开(公告)号：JPH05294990A
公开(公告)日：1993-11-09
申请号：JP12414292
申请日：1992-04-16
申请人： FUJII YOICHI
发明人： FUJII YOICHI , IKEDA YUKARI , YAMAZAKI MITSURU
IPC分类号： A61K39/395 , C07J17/00 , C07K16/00 , C07K17/10 , G01N33/53
摘要： PURPOSE:To provide the novel digoxin derivative comprising a digitoxose whose 3' and 3'' positions have been esterified with succinic acid and useful as a raw material for producing a digoxin-resistant antibody used for the determination of the digoxin by an immunological measuring method useful in the field of clinical examination, etc. CONSTITUTION:The digoxin is dissolved in anhydrous pyridine, mixed with a mixture of acetic anhydride and formic acid under cooling with ice, and subjected to their reaction for 4hr. The reaction solution is mixed with water and extracted with ethyl acetate. The ethyl acetate layer is washed with water, concentrated under vacuum, dissolved in anhydrous pyridine, mixed with succinic anhydride and subsequently heated at 60-70 deg.C for 73hrs. The reaction solution is mixed with water and extracted with ethyl acetate. The ethyl acetate layer is washed with water, concentrated under vacuum, dissolved in methanol, mixed with a 5% aqueous solution of sodium bicarbonate and subsequently heated at 60-70 deg.C. Methanol is distilled away from the reaction solution, and the residue is extracted with ethyl acetate and then purified by a silica gel chromatography to provide the digoxin derivative of the formula [either of R1 and R2 is H and the other is CO(CH2)2COOH].

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