Method for quickly hydrolyzing 6-deoxy-D-allose in tylosin

A technology of tylosin and allose, which is applied in the field of synthesizing antibiotics for livestock and poultry, can solve the problems of difficulty in controlling the degree of side reactions, difficulty in controlling the process, long hydrolysis reaction time, etc., so as to reduce the content and cost of by-products. Low cost and the effect of improving the purity of intermediates

Pending Publication Date: 2020-11-24
NINGXIA TAIYICIN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the harsh hydrolysis conditions of 6-deoxy-D-allose on tylosin lactone, and the bond energy of the glycosidic bond is similar to that of mycosaminoglycan that does not need to be hydrolyzed, in the traditional synthesis process, There have always been problems such as long hydrolysis reaction time and difficulty in controlling the degree of side reactions, which have brought certain difficulties and troubles to the control of subsequent processes
At the same time, because the hydrolysis by-product (fully hydrolyzed tylosactone) is relatively close to des(6-deoxy-D-allose)-tylosin in terms of physical and chemical properties and reactivity, there is also a control on the quality of the finished product. great influence

Method used

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  • Method for quickly hydrolyzing 6-deoxy-D-allose in tylosin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dissolve 30kg of tylosin in 900L of butyl acetate solution, cool down to 2-7°C, add 300L of purified water, adjust the pH of the aqueous phase to 2.5-5.5 with 0.1mol / L hydrochloric acid, and extract for 20 minutes. The organic phase was separated to obtain an aqueous solution of tylosin hydrochloride.

[0032] Dissolve 260g of polymer-dispersed carbon-based nano-solid acid containing sulfonic acid groups in 40L of ethylene glycol, and input it into the primary microreactor at a pressure of 0.08Mpa. Raise the temperature of the reactor to 65°C, circulate for 2 to 4 hours, stop the circulation, and discharge the ethylene glycol solution. The microreactor is rinsed with purified water to complete the immobilization of the polymer dispersed carbon-based nanometer solid acid on the microreaction.

[0033] The temperature of the microreactor loaded with polymer dispersed carbon-based nanometer solid acid was raised to 35° C., and the aqueous solution of tylosin hydrochloride...

Embodiment 2

[0038] Dissolve 150kg of tylosin in 5000L of ethyl acetate solution, cool down to 2-7°C, add 1800L of purified water, adjust the pH of the aqueous phase to 2.5-5.5 with 0.05mol / L hydrochloric acid, and extract for 30 minutes. The organic phase was separated to obtain an aqueous solution of tylosin hydrochloride.

[0039] Dissolve 280g of polymer dispersed carbon-based nanometer solid acid in 60L of ethylene glycol, and feed it into the primary microreactor at a pressure of 0.08Mpa. Raise the temperature of the reactor to 50°C, circulate for 3 to 7 hours, stop the circulation, and discharge the ethylene glycol solution. The microreactor is rinsed with purified water to complete the immobilization of the polymer dispersed carbon-based nanometer solid acid on the microreaction.

[0040]The temperature of the microreactor loaded with polymer dispersed carbon-based nanometer solid acid was raised to 37°C, and the aqueous solution of tylosin hydrochloride was injected at a pressure...

Embodiment 3

[0045] Dissolve 150kg of tylosin in 50L of methyl tert-butyl ether solution, cool down to 2-7°C, add 18L of purified water, and adjust the pH of the aqueous phase to 2.5-5.5 with 0.05mol / L hydrochloric acid. Extract for 30 minutes, and separate the organic phase to obtain an aqueous solution of tylosin hydrochloride.

[0046] 2.8g polymer dispersed carbon-based nanometer solid acid is dissolved in 600ml isopropanol, and is input in the primary microreactor with the pressure of 0.08Mpa. Raise the temperature of the reactor to 55° C., circulate for 5 hours, stop the circulation, and discharge the isopropanol solution. The microreactor is rinsed with purified water to complete the immobilization of the polymer dispersed carbon-based nanometer solid acid on the microreaction.

[0047] The temperature of the microreactor loaded with polymer dispersed carbon-based nanometer solid acid was raised to 43°C, and the aqueous solution of tylosin hydrochloride was injected at a pressure o...

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Abstract

The invention relates to a method for quickly hydrolyzing 6-deoxy-D-allose in tylosin. The method comprises the following steps: immobilizing sulfo-containing carbon-based nano solid acid in a primarymicroreactor with active functional groups, then injecting an aqueous solution of tylosin hydrochloride into the primary microreactor, and carrying out a cyclic reaction, when the residual amount ofthe tylosin is less than 4%, pumping the above-mentioned reaction solution into a secondary microreactor, fully mixing the reaction solution with a halogenated hydrocarbon organic solvent and an alkali solution, and separating out a light phase by using a centrifugal extractor to obtain high-purity 6-deoxy-D-allocatolactone. According to the method, 6-deoxy-D-allose on tylosin lactone molecules can be rapidly and efficiently hydrolyzed, and production efficiency of full-hydrolyzed byproducts is reduced, so that the purposes of optimizing a reaction route of tildipirosin, shortening a reactionperiod, reducing production cost and improving product quality are achieved.

Description

technical field [0001] The invention belongs to the technical field of antibiotic synthesis for poultry and livestock, and specifically relates to a method for synthesizing 6-deoxy-D-allose in an antibiotic intermediate tylosin for poultry and livestock. Background technique [0002] Tildipirosin is a new type of semi-synthetic antibiotic of macrocyclic lactone specially used for animals. It is a broad-spectrum antibacterial drug and is especially sensitive to pathogenic bacteria that cause respiratory diseases in pigs and cattle. The therapeutic effect is very obvious and has a dosage Less, high bioavailability, one-time administration of the whole treatment, low residue and many other advantages. In particular, the current high morbidity and mortality of the respiratory system have become the main problems faced by the global pig and cattle breeding industry. Therefore, Tedirosin has a very wide application prospect. [0003] In the prior art, Tedirosin is a semi-syntheti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/00C07H17/08B01J27/02
CPCC07H1/00C07H17/08B01J27/02
Inventor 赵伯龙于荣刘晓明张智胜赵婷
Owner NINGXIA TAIYICIN BIOTECH CO LTD
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