Antibiotic based on crystalline monohydrate form of 1-carbocephalosporin

专利摘要:
The novel crystalline monohydrate of 7 beta -[2 min -(R)-2 min -phenyl-2 min -aminoacetamido]-3-chloro-3-(1-carbadethia-ce phem)-4-carboxylic acid is a valuable antibiotic and can be prepared from aqueous solutions by adjusting the pH to from 2 to 6.
公开号:SU1731058A3
申请号:SU884356543
申请日:1988-10-05
公开日:1992-04-30
发明作者:Элейн Пасини Кэрол
申请人:Эли Лилли Энд Компани (Фирма)；
IPC主号:

专利说明:

the penny was stirred for 20 minutes. DarcoW G60 carbon black (750 ml, about 250 g) was added to the solution and the resulting suspension was stirred at 24
18.5 cm Buchner funnel containing paper made of fiberglass and filter Hyf1o TO. Filtered solution about ° C 30 min. Suspension Filtered


nitrile (500 ml)
in 1 hour. The resulting suspension was filtered over glass fiber paper and the filter cake was washed with additional acetone.
The substance on the filter cakes LY 163892, which can be used without additional purification).
Water (1.62 L) and hydrochloric acid (12 molar, 43.0 MP) were combined and stirred at 20 ° C. 7j3- / 2 (R) 2 -phenyl 2 -amino-acetamido / -3 was added to the solution. -chloro 3- (1-carba, -1-children-acephaem) -4 carboxylic acid trihydra (200.0 g) and the resulting solution was stirred for 30 minutes. An additional amount of hydrochloric acid (10 ml) was added and the suspension was stirred for 20 minutes. to the solution, charcoal (8.0 g) was added to this solution and the resulting suspension was stirred for 30 minutes. The suspension was filtered through a Hyflo filter aid liner on glass fiber paper (the filter was then washed with 100 ml of water). The filtrate was heated to 45 ° C. 25 min. Triethylamine was slowly added to this filtrate to increase the pH of the solution to 1.8 (during the addition, the temperature of the filtrate was maintained in the range of 45-50 ° C). The solution was seeded with 100 mg of LY 163892 monohydrate, which resulted in suspension. The suspension was stirred for 1 hour pyr 50 ° C. “The addition of triethylamine slowly increased the pH of the suspension to 4.8, the Dann suspension was stirred for another 25 minutes at 50 ° C, then cooled to 25 ° C and stirred for 1 hour. The suspension was filtered through a 24 cm funnel. Buchner fitted with a polypropylene gasket. The filter cake was washed with water (2 ×, 250 ml), then the funnel was closed and the filter cake was under vacuum overnight. This filter cake was placed in a dryer with clean air at 30 ° C for 24 hours and obtained 119.90 g, yield 65.9%, of crystalline monohydrate LY 163892.

权利要求:
Claims (1)
[1]
Invention Formula
eok
having the following x-ray diffraction properties measured for a powder under irradiation with a wavelength of 9 1.541 And And on a copper tube with a nickel filter (Cu: Ni) with the following values of interplanar distances d and relative intensities 1/1
)
Relative intensity 1/1
 5 Q 20 25 JQ
40

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引用文献:

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法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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US10576687A| true| 1987-10-06|1987-10-06|

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