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Green production method for continuously preparing nitrominocycline

A technology for green production of nitrominocycline, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of difficult separation of nitrominocycline and environmental pollution.

Active Publication Date: 2020-03-27
南京恒道医药科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production method of nitrominocycline that is widely used in industry is mainly minocycline nitration method. The problem existing in this process is that the product nitrominocycline is difficult to separate in the reaction system, and the reaction The sulfuric acid used will cause serious environmental pollution and other problems

Method used

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  • Green production method for continuously preparing nitrominocycline
  • Green production method for continuously preparing nitrominocycline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The reaction product is qualitatively and quantitatively detected by high-performance liquid chromatography: octadecylsilane bonded silica gel is used as a filler (4.6mm×150mm, 3μm or a chromatographic column with equivalent performance), and 0.03mol / L disodium hydrogen phosphate solution (Adjust the pH value to 6.3 with phosphoric acid)-acetonitrile (44:56) as the mobile phase; the detection wavelength is 250 nm, and the injection volume is 20 μl.

[0022] Pump sodium nitrite and minocycline into the reaction kettle according to the molar ratio of 10:1; sulfuric acid and minocycline according to the molar ratio of 1:1, heat to the reaction temperature of 35°C, stir vigorously for 5 hours, and the reaction The liquid is pumped into the top of the rotary extraction tower from the bottom of the reaction kettle, and the ethyl acetate solution of isopropylamine is pumped into the countercurrent extraction from the bottom of the rotary extraction tower at the same time, ensur...

Embodiment 2

[0024] Reaction product qualitative and quantitative detection method and operation are all the same as in Example 1, and the implementation steps of changing the reactant molar proportion and each operating parameter are as follows:

[0025] Pump sodium nitrite and minocycline into the reaction kettle according to the molar ratio of 8:1; sulfuric acid and minocycline according to the molar ratio of 20:1, heat to the reaction temperature of 20°C, stir vigorously for 3 hours, and then The liquid is pumped into the top of the rotary extraction tower from the bottom of the reaction kettle, and the ethyl acetate solution of diethylamine is pumped into the countercurrent extraction from the bottom of the rotary extraction tower at the same time, so as to ensure that the flow rate of the reaction liquid pumped into the rotary extraction tower is continuously added diethylamine ethyl acetate 0.5 times of the flow rate of the ester solution, adjust the rotation speed of the rotating di...

Embodiment 3

[0027] Reaction product qualitative and quantitative detection method and operation are all the same as in Example 1, and the implementation steps of changing the reactant molar proportion and each operating parameter are as follows:

[0028] Pump sodium nitrite and minocycline into the reaction kettle according to the molar ratio of 5:1; sulfuric acid and minocycline according to the molar ratio of 15:1; The liquid is pumped into the top of the rotary extraction tower from the bottom of the reaction kettle, and the ethyl acetate solution of triethylamine is pumped into the countercurrent extraction from the bottom of the rotary extraction tower at the same time, so as to ensure that the flow rate of the reaction liquid pumped into the rotary extraction tower is to continuously add triethylamine ethyl acetate 0.3 times of the flow rate of the ester solution, adjust the rotation speed of the rotary disc in the rotary disc extraction tower to 180rpm to fully mix the two phases. ...

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Abstract

The invention relates to a green production method for continuously preparing nitrominocycline. The preparation method comprises the following steps of: feeding minocycline, sodium nitrite and sulfuric acid into a reaction kettle for reaction; then feeding the reaction liquid into the top of a turntable extraction tower from the bottom of the reaction kettle, at the same time, feeding an ethyl acetate solution of organic amine from the bottom of the turntable extraction tower for countercurrent extraction; and adjusting the rotating speed of a turntable in the turntable extraction tower to mixthe two phases, discharging the reaction liquid from the bottom of the turntable extraction tower, discharging the extracted ethyl acetate phase from the top of the turntable extraction tower, concentrating the ethyl acetate phase under reduced pressure, and performing cooling, crystallizing and filtering to obtain the nitrominocycline. The continuous production process of nitration reaction of minocycline and sodium nitrite and separation of nitro minocycline is achieved by adopting the reaction kettle coupled with the turntable tower, so that the reaction product can be timely and continuously separated from the reaction system, low-energy-consumption, simple, rapid and continuous production is achieved, and the yield of the obtained reaction product nitrominocycline is greater than 90%.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a method for producing nitrominocycline by using minocycline and sodium nitrite, and relates to the preparation technology of nitrominocycline, an important intermediate of tigecycline in the field of pharmacy . Background technique [0002] Tigecycline is also known as 9-tert-butylglycylaminominocycline. The original research and development company of tigecycline is Wyeth. It is the first glycamidecycline antibiotic approved for intravenous administration. Tigecycline has a broad antibacterial spectrum, rapid onset and strong antibacterial effect. [0003] Nitrominocycline is an important intermediate in the process of producing tigecycline. At present, the production method of nitrominocycline that is widely used in industry is mainly minocycline nitration method. The problem existing in this process is that the product nitrominocycline is difficult to separate in the rea...

Claims

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Application Information

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IPC IPC(8): C07C237/26C07C231/12
CPCC07C231/12C07C237/26
Inventor 凌岫泉陶义华穆加兵
Owner 南京恒道医药科技股份有限公司
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