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Process for preparing straight-through 6-aminopenicillanic acid

A technology of aminopenicillinic acid and straight-through type, which is applied in the field of preparation of 6-aminopenicillinic acid, can solve the problems of unfavorable product quality control, unsatisfactory yield, long operation time, etc., and achieve low cost and high product yield High and fast degreasing effect

Inactive Publication Date: 2010-06-16
NORTH CHINA PHARMA COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the resin can also adsorb penicillin while adsorbing esters. Even if the resin is regenerated, some penicillins cannot be successfully resolved and recovered, so this method still has the problem of unsatisfactory yield.
In addition, the existing method also has the following deficiencies: one, the alkaline solution extraction reagents used in the existing technology are potassium carbonate or sodium carbonate solution, so the cost is higher
Two, the stripping process is mainly realized by intermittent mixing and clarification tank operation, and the operation time of this method is long (about 7 hours for one batch); three, the addition of alkali solution is mainly carried out by experience, which is not conducive to product quality control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] a. The penicillin fermented liquid is filtered, acidified and extracted to obtain a butyl acetate solution of penicillin with a potency of 6-120,000 u / ml, that is, a BA, which is washed with water to obtain a washed BA.

[0027] b. Add the water-washed BA and the prepared ammonia solution of 1-5% (w / w) into the pod machine through their respective pipelines. In the pod machine, countercurrent stripping occurs while mixing and reacting while separating. The reading of the online pH detector at the outlet of the phase will automatically feedback and adjust the amount of ammonia water added, so that the pH of the heavy phase RB is within the required range of 6.5-7.5. The export titer of the light phase reaches 0, and the titer of the heavy phase is about 300,000 u / ml. The extraction yield is 99.5%.

[0028] c. The heavy phase enters a buffer tank, and directly enters a degreasing tower (a vacuum refining tower) for degreasing operation. The heavy phase enters the tower ...

Embodiment 2

[0032] Penicillin fermentation liquid is filtered, acidified and extracted to obtain butyl acetate solution of penicillin with a titer of 92,000 u / ml, that is, primary BA, and the primary BA is mixed with a concentration of 1-5% (w / w) bicarbonate The ammonium aqueous solution is added to the TA machine through its own pipeline, and the countercurrent stripping process of mixing, reacting and separating occurs in the TA machine, and the ammonium bicarbonate is automatically adjusted by feedback through the online pH detector at the outlet of the heavy phase of the TA machine. The adding amount of the aqueous solution makes the pH of the heavy phase RB between the required range of 6.0-6.5. The export titer of the light phase reaches 0, and the RB titer of the heavy phase is around 250,000 u / ml. The stripping yield is 99.7%. The heavy phase enters a buffer tank and directly enters the degreasing tower (a falling film tube) for degreasing operation. The heavy phase RB and a sma...

Embodiment 3

[0035]Penicillium fermentation broth is filtered, acidified, and butyl ester is concentrated and extracted to obtain a titer of 70,000 to 100,000 units of butyl penicillinate extract (i.e. one BA), add activated carbon at 40-100g / billion units, and add activated carbon at -20- Stir at 10°C for 20-60 minutes, filter; to remove part of the colored impurities in primary BA, filter, add 9-12% potassium carbonate solution to the filtrate at 1.0-1.5 liters / billion units, stir, stand still and separate phases, Back-extraction to obtain penicillin potassium aqueous solution (RB), so that the RB titer is controlled at 450,000-550,000 units. The heavy phase enters a buffer tank and directly enters the degreasing tower (a falling film tube) for degreasing operation. The heavy phase RB and a small amount of steam enter the tower from the top of the tower, and the interlayer in the tower wall passes through low-pressure steam or hot water. The water temperature is between 40-70 ° C. The ga...

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Abstract

The invention discloses a process for preparing straight-through 6-aminopenicillanic acid, which comprises the following steps: a, filtering and acidizing penicillin fermentation solution, extracting the penicillin fermentation solution by using butanol, and concentrating and decoloring the extract to obtain butyl ester extracting solution of penicillin; b, back extracting the butyl ester extracting solution of the penicillin by using alkali solution to obtain brine solution of penicillin (heavy phase or RB for short); c, continuously injecting the brine solution of the penicillin into a degreasing tower in a vacuum pressure reduction state to convert the butyl ester into a gas phase from the brine solution of the penicillin, discharging the degreased brine solution of the penicillin out of a pressure reduction system from the bottom of the tower to a storage tank with a cooling device, and cooling the degreased brine solution of the penicillin for later use; and d, performing enzymatic conversion on the degreased brine solution of the penicillin, then adding 6-APA crystal seeds into the solution, growing the crystals, crystallizing the solution, and drying the crystals.

Description

technical field [0001] The invention relates to a preparation method of pharmaceutical raw materials, in particular to a preparation method of 6-aminopenicillin alkanoic acid. Background technique [0002] 6-aminopenicillin alkanoic acid is referred to as 6-APA. With 6-APA as the core, it can be condensed with different side chains to prepare β-lactam semi-synthetic antibiotics. β-lactam semi-synthetic antibiotics are widely used in clinic because of their definite curative effect and less toxic side effects. 6-APA is an important raw material for the production of semi-synthetic antibiotic intermediates of β-lactams. The traditional preparation method of 6-APA is usually a double crystallization process, that is, first azeotroping penicillin saline solution and butanol, crystallization, and drying to prepare penicillin potassium salt industrial powder; Transformation and crystallization give 6-APA. The disadvantages of this method are large loss of yield, low yield of f...

Claims

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Application Information

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IPC IPC(8): C07D499/42C12P37/00
Inventor 李秋元王分良王华瑞刘丹吴立强刘华王欣刘亚红
Owner NORTH CHINA PHARMA COMPANY
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