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A kind of preparation method of oxytetracycline hydrochloride

A technology of oxytetracycline hydrochloride and oxytetracycline hydrochloride, which is applied in the field of preparation of oxytetracycline hydrochloride, can solve the problems of insufficient utilization of cosolvent and hydrochloric acid methanol, increased methanol consumption, and high methanol consumption, so as to reduce the amount of solid waste, The effect of reducing production costs and reducing the number of recycling

Active Publication Date: 2019-12-20
盐城市大丰区天生联合药业有限公司
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are following problems in the existing technique in this process: 1. yield is low, and cost is high, and part oxytetracycline unreacted generates oxytetracycline hydrochloride or generates other oxytetracycline compound impurity after reaction, and utilization rate is low, simultaneously its It is discharged in the form of waste liquid or waste residue, which brings environmental protection problems; 2. The consumption of methanol is high, and part of the methanol will inevitably escape in the form of steam during the recovery process of the mother liquor, which will increase the consumption of methanol and pollute the atmosphere; 3. The co-solvent and Methanol hydrochloride is not fully utilized and the loss is large

Method used

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  • A kind of preparation method of oxytetracycline hydrochloride
  • A kind of preparation method of oxytetracycline hydrochloride

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preparation example Construction

[0023] A kind of preparation method of oxytetracycline hydrochloride of the present invention, it comprises the steps:

[0024] One, get raw material oxytetracycline and ethanol and put into the first reactor in proportion (kg / L) 1:3.5, after heating up and distilling for a period of time, cool to room temperature, then the material in the first reactor is centrifuged through centrifuge, Obtain oxytetracycline wet product with water content lower than 0.1%;

[0025] 2. Put calcium chloride and methanol into the second reaction kettle, stir and dissolve to obtain a calcium chloride methanol solution, then add the wet product of oxytetracycline in step 1 to the second reaction kettle, stir, slightly heat, until all After dissolving, add a small amount of activated carbon, stir, and filter to obtain oxytetracycline methanol solution. After the oxytetracycline methanol solution is cooled, add hydrogen chloride methanol solution, stir and crystallize, cool, filter, and wash the fil...

Embodiment 1

[0038] (1) get raw material oxytetracycline 1000kg, ethanol 4000L is sent in the first reaction kettle, ethanol is distilled out about 2000L by heating, is cooled to room temperature, centrifuges, obtains the oxytetracycline alkali wet product that water content is lower than 0.1%.

[0039] (2) Take the wet product of oxytetracycline from step (1), 4000L of methanol, and 100kg of calcium chloride, put them into the second reaction kettle sink, stir and dissolve at about 30°C until clarified, add 15kg of activated carbon, continue to stir for 10 minutes, filter, and the filtrate Use methanol equivalent to 76kg of hydrogen chloride to form a salt, cool the system to ≤0°C, centrifuge, and dry to obtain a finished product, and transport the mother liquor to a liquid storage tank.

[0040] (3) Take the wet product of oxytetracycline in step (1), put 4000L of mother liquor into the second reaction kettle, stir and dissolve at about 30°C until clarified, add 15kg of activated carbon, ...

Embodiment 2

[0046] (1) get raw material oxytetracycline 1000kg, ethanol 4000L is sent in the first reaction kettle, ethanol is distilled out about 2000L by heating, is cooled to room temperature, centrifuges, obtains the oxytetracycline alkali wet product that water content is lower than 0.1%.

[0047] (2) Take the wet product of oxytetracycline in step (1), 4000L of methanol, hydrochloric acid methanol equivalent to 35kg of hydrogen chloride, put it into the second reaction kettle sink, stir and dissolve at about 30°C until clear, add 15kg of activated carbon, continue to stir for 10 minutes, and filter , the filtrate is salted with methanol hydrochloric acid equivalent to 41kg of hydrogen chloride, the temperature of the system is lowered to ≤0°C, centrifuged, and dried to obtain the finished product, and the mother liquor is transported to the liquid storage tank.

[0048](3) Take the wet product of oxytetracycline in step (1), put 4000L of mother liquor into the second reaction kettle,...

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Abstract

The invention provides a preparation method of oxytetracycline hydrochloride. A method of co-boiling raw materials and alcohol for dewatering is adopted to remove moisture in oxytetracycline, dissolved quantity of oxytetracycline hydrochloride in mixed liquid of subsequently-generated methanol and a little of water is reduced, yield of oxytetracyline hydrochloride is increased, subsequently-generated oxytetracycline impurities are reduced, mother liquid can be directly reused without distillation and purification of methanol therein, and consumption of methanol and calcium chloride is reduced. The preparation method has the advantages that yield is increased, cost is lowered, and environment pollution is reduced.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a preparation method of oxytetracycline hydrochloride. Background technique [0002] Oxytetracycline hydrochloride, also known as oxytetracycline hydrochloride, oxytetracycline hydrochloride, or oxytetracycline hydrochloride, is an antibiotic widely used in humans and animals, and is clinically used to treat various diseases, such as rickettsiasis, including Epidemic typhus, endemic typhus, scrub typhus; infection caused by Mycoplasma pneumoniae; chlamydial infection, including psittacosis, venereal lymphoid edema, nonspecific urethritis, salpingitis, and trachoma; relapsing fever; Brucella disease; cholera; plague and tularemia, etc. The dosage forms of oxytetracycline hydrochloride are tablets, capsules, powders, eye drops and ointments. [0003] The existing production process of oxytetracycline hydrochloride is to select a certain co-solvent, dissolve, absorb and filter t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/12C07C237/26
CPCC07C231/12C07C237/26
Inventor 陈隽楼彭广荣韦俊
Owner 盐城市大丰区天生联合药业有限公司
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