A kind of method that solvent crystallization method prepares ampicillin sodium
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A technology of ampicillin sodium and ampicillin acid, applied in the direction of organic chemistry, can solve the problems of uncontrollable crystallization speed, uneven particle size distribution, troublesome solvent recovery, etc., and achieve larger crystal nuclei, uniform particle size distribution, and easy recycling The effect of using
Active Publication Date: 2016-08-24
山东安信制药有限公司
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The disadvantage of this method is also that the crystallization speed cannot be controlled, resulting in fast crystallization of the product, causing n-butanol to be wrapped in it, high dissolved residue, fine powder, uneven particle size distribution, and difficult to pack
Moreover, ampicillin amine salt needs to be dehydrated with anhydrous magnesium sulfate, which is cumbersome to operate and troublesome for solvent recovery.
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Embodiment 1
[0022] (1) Preparation of sodium isooctanoate: Dissolve 45 kg of sodium isooctanoate in 90 liters of methanol, filter the resulting solution aseptically into a crystallization tank, rinse the pipeline with 50 liters of dichloromethane, and filter the lotion Put it into the storage tank in the crystallization area for standby;
[0023] (2) Preparation of ampicillin amine salt: pour 200 liters of dichloromethane into the batching tank, cool to 15°C through the jacket, add 100 kilograms of ampicillin trihydrate, then drop 45 liters of diisopropylamine, ampicillin The acid gradually dissolves and becomes clear, and the resulting clear liquid is aseptically filtered into a crystallization tank, and the pipeline is washed with 50 liters of dichloromethane;
[0024] (3) The sodium isooctanoate solution is transferred in the crystallization tank, and 450 liters of dichloromethane is added; Then add 0.1 kg of ampicillin sodium seed crystals, and grow crystals statically for 30 minutes;...
Embodiment 2
[0030] (1) Preparation of sodium isooctanoate: Dissolve 45 kg of sodium isooctanoate in 90 liters of methanol, filter the resulting solution aseptically into a crystallization tank, rinse the pipeline with 45 liters of dichloromethane, and filter the lotion Put it into the storage tank in the crystallization area for standby;
[0031] (2) The preparation of ampicillin amine salt: control temperature at 15 ℃, 100 kilograms of ampicillin trihydrates are joined in 220 liters of dichloromethane, drop 45 liters of diisopropylamine, ampicillin acid gradually dissolves and becomes clear, and Gained clear liquid is aseptically filtered into the crystallization tank, and the pipeline is washed with 40 liters of dichloromethane;
[0032] (3) The sodium isooctanoate solution is transferred in the crystallization tank; Add 420 liters of dichloromethane, then add 0.1 kg of ampicillin sodium seed crystals, and grow crystals statically for 20 minutes, until the feed liquid becomes muddy and ...
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Abstract
The invention discloses a method for preparing ampicillin sodium by a menstruum crystallization method. The method comprises the following steps: firstly, dissolving sodium 2-ethylhexanoate into methanol, controlling the temperature to 15 DEG C, adding ampicillin acid into dichloromethane, and dripping diisopropylamine for a dissolution reaction; adding a sodium 2-ethylhexanoate solution into a crystallization tank, then adding a dichloromethane liquation agent in a flowing manner, and adding a seed crystal for growing crystals in a standing manner; then adding the dichloromethane liquation agent for crystallization; controlling the crystallization temperature to 20-25 DEG C; controlling the flowing acceleration of the liquation agent to 100 ml / h; after the crystallization reaction is completed, discharging materials, filtering the discharged materials, and drying the filtered materials to obtain the ampicillin sodium. According to the method, the methanol solvent, in which the ampicillin sodium is easy to dissolve, is selected for use, and then the dichloromethane solvent is used for dissolving out products, so that the crystallization speed of the product can be controlled; in addition, measures of adding the seed crystal for growing the crystal, controlling the dissolving temperature and the crystallization temperature, controlling the flowing acceleration of the liquation agent and the like are taken, so that the crystallization speed can be controlled, the crystal nucleus of the product are enlarged and uniform, the product purity is high, the dissolving residue is low, and the quality is stable.
Description
technical field [0001] The invention relates to a preparation method of ampicillin sodium, which belongs to the technical field of medicine. Background technique [0002] Ampicillin sodium is the first generation of broad-spectrum semi-synthetic penicillin, which was developed by Pfizer in 1962 and launched in 1965. With the continuous development of synthetic technology, penicillin has now developed to the second and third generation Semi-synthetic penicillin. As the first generation of semi-synthetic penicillin, ampicillin sodium has the characteristics of broad spectrum, low toxicity, high efficiency and low cost. It can be used for intramuscular injection or intravenous injection. It is widely used to treat upper and lower respiratory tract infections, gastrointestinal tract infections, urinary tract infections, skin and soft tissue infections, meningitis, sepsis, endocarditis, etc. caused by sensitive bacteria. [0003] At present, there are three methods for produci...
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