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1. 发明授权

US3929993A Process for removing copper from copper-containing bleomycin group antibiotics 失效
标题翻译：从含铜博莱霉素组抗生素中去除铜的方法
公开(公告)号：US3929993A
公开(公告)日：1975-12-30
申请号：US33068673
申请日：1973-02-08
申请人： NIPPON KAYAKU KK
发明人： TAKITA TOMOHISA , FUJII AKIO , MURAOKA YASUHIKO , MIZUGUCHI SHIGERU , UMEZAWA HAMAO
IPC分类号： C07H15/26 , C07D277/56 , C07G11/00 , C07K9/00 , A61K37/00
CPC分类号： C07K9/003
摘要： A copper-free form of phleomycin-bleomycin group antibiotics with very small residual copper content and unreduced antitumor activity may be obtained in high yields by contacting an aqueous solution containing a copper-containing form of said antibiotics with a non-ionexchangeable macroreticular resin to allow said antibiotics to be adsorbed on the resin, contacting the resin with an aqueous solution containing a chelating agent to release copper from said antibiotics, and then with an organic solvent containing water to elute the adsorbed antibiotics.
摘要翻译：通过使含有含铜形式的所述抗生素的水溶液与非可离子交换的大网状树脂接触，可以以高产率获得具有非常小的残余铜含量和未降低的抗肿瘤活性的无腐蚀形式的腐草霉素 - 博来霉素组抗生素，以允许所述抗生素被吸附在树脂上，使树脂与含有螯合剂的水溶液接触，以从所述抗生素中释放铜，然后用含水的有机溶剂洗脱吸附的抗生素。

2. 发明授权

KR810001407B1 PROCESS FOR PREPARING 3-((S)-V-PHENYL ETHYL AMINO)-PROPYLAMINOBLEOMYCIN NON-TOXIC SALT THEREOF 失效
公开(公告)号：KR810001407B1
公开(公告)日：1981-10-20
申请号：KR780001991
申请日：1978-06-28
申请人： NIPPON KAYAKU KK
发明人： TAKITA TOMOHISA , FUJII AKIO , FUKUOKA TAKEYO , UMEZAWA HAMAO , YOSIOKA OSAMU , MURAOKA YASUHIKO
IPC分类号： A61K31/505 , C07H15/26 , C07C103/52
摘要： Title compd.(I), useful as antibiotic, was prepd. by reaction of N-[(S)-1'-phenylethyl -1,3-diaminopropane and reactive derivs. of bleomycinic acid in the solvent. Thus, bleomycinic acid 1.5 g was dissolved in the NK 631 dihydrochloride water soln. 40 ml, stirred, pH was adjusted with 0.1 N-NaOH aq. soln. to 0.8-5.5, and then NEPIS 800 mg was added at 26oC. After 30 min, amino compd. 1.8 g was dissolved in the reaction mixt., left for 20 hr at 26oC, cold acetone 60 ml was added, filtered and then washed with acetone to give NK 631 dihydrochloride 932 mg.

3. 发明专利

CS205127B2 PROCESS FOR PREPARING 3-/S/-1'-PHENYLETHYLAMINO-PROPYLAMINOBLEOMYCINE 未知
公开(公告)号：CS205127B2
公开(公告)日：1981-04-30
申请号：CS592679
申请日：1979-08-30
申请人： NIPPON KAYAKU KK
发明人： TAKITA TOMOHISA , FUJII AKIO , FUKUOKA TAKEYO , MURAOKA YASUHIKO , YOSHIOKA OSAMU , UMEZAWA HAMAO
IPC分类号： C07H15/26

4. 发明专利

DE3008359A1 未知
公开(公告)号：DE3008359A1
公开(公告)日：1980-09-18
申请号：DE3008359
申请日：1980-03-05
申请人： NIPPON KAYAKU KK
发明人： FUJII AKIO , FUKUOKA TAKEYO , MURAOKA YASUHIKO , TAKITA TOMOHISA , UMEZAWA HAMAO
IPC分类号： C07K9/00 , C07H15/26 , A61K31/495

5. 发明专利

DE2307543A1 未知
公开(公告)号：DE2307543A1
公开(公告)日：1973-08-30
申请号：DE2307543
申请日：1973-02-15
申请人： NIPPON KAYAKU KK
发明人： TAKITA TOMOHISA , FUJII AKIO , MURAOKA YASUHIKO , MIZUGUCHI SHIGERU , UMEZAWA HAMAO
IPC分类号： C07H15/26 , C07D277/56 , C07G11/00 , C07K9/00 , C07C103/52
摘要： A copper-free form of phleomycin-bleomycin group antibiotics with very small residual copper content and unreduced antitumor activity may be obtained in high yields by contacting an aqueous solution containing a copper-containing form of said antibiotics with a non-ionexchangeable macroreticular resin to allow said antibiotics to be adsorbed on the resin, contacting the resin with an aqueous solution containing a chelating agent to release copper from said antibiotics, and then with an organic solvent containing water to elute the adsorbed antibiotics.

6. 发明专利

DK157081C 未知
公开(公告)号：DK157081C
公开(公告)日：1990-04-09
申请号：DK299578
申请日：1978-06-30
申请人： NIPPON KAYAKU KK
发明人： TAKITA TOMOHISA , FUJII AKIO , FUKUOKA TAKEYO , MURAOKA YASUHIKO , YOSHIOKA OSAMU , UMEZAWA HAMAO
IPC分类号： C07K9/00 , C07H15/26
摘要： Novel 3-[(S)-1'-phenylethylamino]propylaminobleomycin obtained by reacting a reactive derivative of the carboxyl group of bleomycinic acid with N-[(S)-1'-phenylethyl]-1,3-diaminopropane, a non-toxic salt of said novel bleomycin, and a method for producing the novel bleomycin. Because of much reduction in the side effect causing pulmonary fibrosis, the novel bleomycin is more useful than a commercial bleomycin complex which gives rise to said undesirable side effect.

7. 发明专利

CH634582A5 3-((S)-1'-PHENYLAETHYLAMINO)-PROPYLAMINOBLEOMYCIN, VERFAHREN ZU SEINER HERSTELLUNG UND DIESE VERBINDUNG ENTHALTENDES ARZNEIMITTEL. 未知
公开(公告)号：CH634582A5
公开(公告)日：1983-02-15
申请号：CH707678
申请日：1978-06-29
申请人： NIPPON KAYAKU KK
发明人： TAKITA TOMOHISA , FUJII AKIO , FUKUOKA TAKEYO , MURAOKA YASUHIKO , YOSHIOKA OSAMU , UMEZAWA HAMAO
IPC分类号： C07K9/00 , C07H15/26 , A61K31/71

8. 发明专利

GB866425A The antibiotic variotin and the production thereof 未知
公开(公告)号：GB866425A
公开(公告)日：1961-04-26
申请号：GB1179059
申请日：1959-04-07
申请人： JAPAN ANTIBIOTICS RES ASS , NIPPON KAYAKU KK
发明人： SUMIKI YUSUKE , UMEZAWA HAMAO , YONEHARA HIROSHI , YAMANAKA KUNIO , TAKITA TOMOHISA , AKITO EIICHIRO , VENO KEIHEI , TAHARA KOSAKU
摘要： A new antibiotic variotin active against fungi is obtained by cultivating a strain of Paecilomyces varioti Bainier var antibioticus (e.g. ATCC 13435, or a mutant thereof) under aerobic and preferably submerged conditions in an aqueous nutrient medium containing a source of carbon, nitrogen and mineral salts. The temperature is 20 to 40 and preferably 25 DEG C., the pH 6,0 and the duration 2 to 6 days for submerged cultivations. Suitable carbon sources are sucrose, glucose, fructose, mannose, glycerine, starch, mannan, malt sugar, xylose, lactose and molasses. Nitrogen sources are sodium nitrate, ammonium nitrate, calcium nitrate, ammonium sulphate, soybean meal, peanut meal, cottonseed meal, meat extract, peptone, corn steep liquor and yeast extract. Mineral Mineral salts are sodium chloride, potassium dihydrogen phosphate, potassium chloride, magnesium sulphate and ferrous sulphate. Variotin is isolated by the solvent extraction of (a) whole broth (b) the clarified broth and (c) the separated mycelium. In the case of (a) and (b), there is used a water-immiscible organic solvent such as butanol, amyl alcohol, methyl isobutyl ketone, benzene, chloroform, ethyl acetate, butyl acetate and carbon tetrachloride. In the case of (c), the mycelium is extracted with a water-immiscible solvent such as methanol, the solvent removed and the residue extracted with the water-immiscible solvent. Further purification is by means of countercurrent distribution using 70% methanol and carbon tetrachloride (1 : 1). Variotin is a colourless oil with ester-like fragrance, scarcely soluble in water, petroleum ether and ligroin; soluble in methanol, ethanol, butanol, amyl alcohol, ethyl acetate, butyl acetate, acetone, chloroform, glycerol and others; [a ]2D8 = -5,68 DEG (C = 1,0% methanol); contains C=67,35%, H=8,58%, N=4,16% and O=19,91%; in methanol shows maximum absorption in ultraviolet at 318-324 mm (E 1% 1 cm.=1198); in infra red shows maximum absorption at 3460, 3100, 2950, 2880, 1740, 1670, 1600, 1485, 1465, 1430, 1350, 1310, 1260, 1190, 1160, 1125, 1075, 1065, 1025, 1005, 970, 935, 885, 865, 840, 800 and 715 cm-1. Variotin is unstable especially in alkaline solution, more stable at pH 4 to 7,0 and in organic solvents such as butyl acetate, methanol, carbon tetrachloride and 75% aqueous ethanol. Stability is enhanced by the addition of 0,001 to 0,1% of (a) an antioxident such as hydroxyquinone, resorcin, butylhydroxyanisole or butyl hydroxytoluene, and/or(b) a chelating agent such as 8-hydroxyquinoline, 2,3-dimercaptopropanol or ethylene diamine tetraacetic acid or its salts. Variotin may be used medicinally (see Group VI).ALSO:Therapeutic preparations comprise the antifungal antibiotic variotin (see Group IV (b)), in the form of an ointment, solution, suspension, powder or suppository. It is stabilized by (a) dissolving in an organic solvent, e.g. butyl acetate, methanol, carbon tetrachloride or 75% aqueous, (b) the addition of 0.001 to 0.1% of at least one antioxidant selected from hydroxy quinone, 1,3-dihydroxybenzene, 2- or 3-t-butyl-4 - hydroxyanisole or 3,5 - di - tert. - butyl - 4 - hydroxytoluene and/or at least one of the chelating - agents 8 - hydroxyquinoline, 2,3 - dimercaptopropanol, ethylenediamine tetraacetic acid and its salts. Examples are given of ointment bases (e.g. polyethylene glycol and cetanol) containing such stabilizers.

9. 发明专利

CS205126B2 PROCESS FOR PREPARING 3-/S/-1-PHENYLETHYLAMINO-PROPYLAMINOBLEOMYCIN AND NON-TOXIC SALT THEREOF 未知
公开(公告)号：CS205126B2
公开(公告)日：1981-04-30
申请号：CS430178
申请日：1978-06-29
申请人： NIPPON KAYAKU KK
发明人： TAKITA TOMOHISA , FUJII AKIO , FUKUOKA TAKEYO , MURAOKA YASUHIKO , YOSHIOKA OSAMU , UMEZAWA HAMAO
IPC分类号： C07H15/26 , A61K31/70 , A61K31/7028 , A61P35/00

10. 发明专利

DE2828933A1 未知
公开(公告)号：DE2828933A1
公开(公告)日：1979-01-04
申请号：DE2828933
申请日：1978-06-30
申请人： NIPPON KAYAKU KK
发明人： TAKITA TOMOHISA , FUJII AKIO , FUKUOKA TAKEYO , MURAOKA YASUHIKO , YOSHIOKA OSAMU , UMEZAWA HAMAO
IPC分类号： C07K9/00 , C07H15/26 , A61K31/71
摘要： Novel 3-[(S)-1'-phenylethylamino]propylaminobleomycin obtained by reacting a reactive derivative of the carboxyl group of bleomycinic acid with N-[(S)-1'-phenylethyl]-1,3-diaminopropane, a non-toxic salt of said novel bleomycin, and a method for producing the novel bleomycin. Because of much reduction in the side effect causing pulmonary fibrosis, the novel bleomycin is more useful than a commercial bleomycin complex which gives rise to said undesirable side effect.

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