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Preparation method of chlorinated terramycin

The technology of chloroxytetracycline and oxytetracycline is applied in the field of preparation technology of chloroxytetracycline, can solve the problems of large environmental harm, large toxic and side effects, low reaction yield and the like, and achieves low toxic and side effects, The effect of less waste residue and less dosage

Inactive Publication Date: 2017-07-14
扬州联博药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually the production process of oxytetracycline chloride is: add oxytetracycline oxytetracycline into anhydrous methanol, add N-chloroacetanilide under low temperature stirring, and react to form oxytetracycline chloride and acetanilide, and oxytetracycline chloride becomes crystals Precipitate, filter out oxytetracycline chloride, and recover methanol from the mother liquor. This process has large toxic and side effects, great environmental hazards, low reaction yield, and more waste residues

Method used

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  • Preparation method of chlorinated terramycin

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Effect test

Embodiment 1

[0019] A preparation method of oxytetracycline, comprising the following steps:

[0020] 1) Add 500mL of methanol to a 1000mL reactor, control the temperature at 10-15°C, add 60g of oxytetracycline into the reactor and stir; after fully stirring for 1 hour, cool down to 5°C, add 30g of N-chloro Succinimide, stirred for 1h;

[0021] 2) Filter and separate the above materials, wash them with methanol, and discharge them after suction filtration for 30 minutes;

[0022] 3) The product obtained in step 2) was dried in a drying oven to finally obtain 58.83 g of oxytetracycline, an important intermediate of doxycycline, with a yield of 98%.

Embodiment 2

[0024] A preparation method of oxytetracycline, comprising the following steps:

[0025] 1) Add 5L of methanol to a 10L reactor, control the temperature at 10-15°C, add 0.6kg of oxytetracycline into the reactor and stir; after stirring for 1 hour, cool down to 0°C, and add 0.3kg of N - Chlorosuccinimide, stirred for 1h;

[0026] 2) Inject step 1) into the centrifuge for spinning, and wash with methanol, and discharge the material after spinning for 30 minutes;

[0027] 3) The product obtained in step 2) was dried in a blast drying oven to finally obtain 0.57 kg of oxytetracycline, an important intermediate of doxycycline, with a yield of 95%.

Embodiment 3

[0029] A preparation method of oxytetracycline, comprising the following steps:

[0030] 1) Add 500L of methanol to a 1000L reactor, control the temperature at 10-15°C, add 60kg of oxytetracycline into the reactor for stirring, stir thoroughly for 1 hour, cool down to 0°C and add 30kg of N-chloro Succinimide, stirred for 1h;

[0031] 2) Inject step 1) into the filter press for pressure filtration, and discharge after 1 hour of pressure filtration;

[0032] 3) The product obtained in step 2) was dried by an airflow drying system to finally obtain 59.33 kg of oxytetracycline, an important intermediate of doxycycline, with a yield of 98.9%.

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Abstract

The invention discloses a preparation method of chlorinated terramycin, comprising the following steps: 1) adding methanol into a reactor with mechanical agitation, controlling temperature to 10-15 DEG C, adding terramycin into the reactor, stirring and cooling and adding N-chlorosuccinimide, fully stirring and reacting for 1h, and precipitating out crystals after the reaction; 2) injecting a mixture obtained in the step 1) into filtering equipment and filtering, washing with methanol, and discharging after 30 min; and 3) drying a product obtained in the step 2) through drying equipment. By the preparation method of chlorinated terramycin, use amount of the reactant N-chlorosuccinimide is smaller, toxic and side effect is low, and reaction yield is increased and can reach 95%. Therefore, less waste residue is produced, and the method has good practicality.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a preparation process of oxytetracycline chloride. Background technique [0002] Oxytetracycline chloride is an important intermediate product in the production of doxycycline hydrochloride, which is prepared by chlorination of oxytetracycline and used to prepare 11α-chloro-6-methoxycycline, while 11α-chloro -6-Methoxycycline is used in the production of doxycycline hydrochloride. Doxycycline hydrochloride is a good antibacterial drug. In addition, this drug is also widely used in veterinary medicine to treat infections caused by various germs. It is mainly used to treat respiratory tract, urinary tract and biliary tract infections caused by sensitive bacteria. At present, the market of doxycycline is relatively considerable, and the market demand is very large. [0003] [0004] 11α-chloro-6,12 hemiketal oxytetracycline (referred to as oxytetracycli...

Claims

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Application Information

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IPC IPC(8): C07D307/00
CPCC07D307/00
Inventor 陆波苏令倪再欣
Owner 扬州联博药业有限公司
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