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Method for preparing high-quality tilmicosin through low-quality tylosin

A technology of tylosin and tilmicosin, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve problems such as non-compliance with the requirements of the pharmacopoeia, and achieve easy separation, recyclability, economical and environmental protection. Operation, the effect of saving the cost of raw materials

Inactive Publication Date: 2016-07-20
HEZE CITY FANGMING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the D component exceeds 3.5%, the tilmicosin single impurity exceeds 3.0%, which does not meet the requirements of the Pharmacopoeia, and there is currently no effective method for separating tilmicosin impurities

Method used

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  • Method for preparing high-quality tilmicosin through low-quality tylosin

Examples

Experimental program
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Effect test

example 1

[0009] Example 1: Add 110ml of isoamyl acetate and 150ml of water to a 500ml reaction bottle and stir to dissolve 40g of tylosin tartrate. After complete dissolution, adjust the pH to 11 with 30% sodium hydroxide, stir for 10 minutes, and let stand to separate layers. Raise the temperature of the oil phase to 40°C, add 5.36g of 3,5-dimethylpiperidine at one time and stir, continue to heat up to 58°C, and slowly add the formic acid / isoamyl acetate mixture (2.52g formic acid, isoamyl acetate 13.34ml) was raised to 65°C for 4h, then lowered to 40°C. Add 150ml of water, adjust the pH to 2.5 with 15% hydrochloric acid, stir for 20 minutes and let stand to separate layers. The water phase is adjusted to PH=1.56. Maintain at 40°C for 60 minutes, and adjust the pH to 6 with 30% sodium hydroxide. Add 7.0g of Beta molecular sieves, stir at 45°C for 40min, and filter with suction. Slowly add 30% sodium hydroxide dropwise to the filtrate at 40°C to adjust the pH to 12, stir for 1h with...

example 2

[0010] Example 2: Add 115ml of isoamyl acetate and 160ml of water into a 500ml reaction bottle and stir to dissolve 40g of tylosin tartrate. After complete dissolution, adjust the pH to 11 with 30% sodium hydroxide, stir for 20 minutes, and let stand to separate layers. Raise the temperature of the oil phase to 40°C, add 5.37g of 3,5-dimethylpiperidine at one time and stir, continue to heat up to 58°C, and slowly add the formic acid / isoamyl acetate mixture (2.53g formic acid, isoamyl acetate 13.20ml) was raised to 65°C for 4.5h, then lowered to 40°C. Add 150ml of water, adjust the pH to 2.5 with 15% hydrochloric acid, stir for 20 minutes and let stand to separate layers. The water phase is adjusted to PH=1.56. Maintain at 40°C for 60 minutes, and adjust the pH to 6 with 30% sodium hydroxide. Add 7.5g Beta molecular sieves, stir at 47°C for 40min, filter with suction, slowly add 30% sodium hydroxide dropwise at 40°C to adjust the pH to 12, stir for 1h with suction, filter wi...

example 3

[0011] Example 3: Add 110ml of isoamyl acetate and 150ml of water into a 500ml reaction bottle and stir to dissolve 40g of tylosin tartrate. After complete dissolution, adjust the pH to 11 with 30% sodium hydroxide, stir for 10 minutes, and let stand to separate layers. Raise the temperature of the oil phase to 40°C, add 5.36g of 3,5-dimethylpiperidine at one time and stir, continue to heat up to 58°C, and slowly add the formic acid / isoamyl acetate mixture (2.52g formic acid, isoamyl acetate 13.30ml) was raised to 65°C for 5h, then lowered to 40°C. Add 160ml of water, adjust the pH to 2.5 with 15% hydrochloric acid, stir for 20 minutes and let stand to separate layers. The water phase is adjusted to PH=1.56. Maintain at 40°C for 60 minutes, and adjust the pH to 6 with 30% sodium hydroxide. Add 7.3g Beta molecular sieves, stir at 50°C for 40min, filter with suction, slowly add 30% sodium hydroxide dropwise to the filtrate at 40°C to adjust the pH to 12, stir for 1h with suct...

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Abstract

The invention belongs to the technical field of pharmaceuticals, and discloses a method for synthesizing tilmicosin through low-quality tylosin. The method comprises the steps that tylosin tartrate and 3,5-dimethylpiperidine are subjected to an amination reaction by taking isoamyl acetate as solvent under the certain acidity and temperature conditions, acidic hydrolysis is conducted, hydrolysate passes through a Beta molecular sieve, impurities produced by a D component in tylosin are adsorbed, alkali adjustment and crystallization are conducted, and high-quality tilmicosin is obtained. According to the method for synthesizing tilmicosin through low-quality tylosin, low-quality tylosin tartrate can be adopted, the quality requirement of the raw material is lowered, the raw material cost is reduced, the applied Beta molecular sieve is easy to separate and capable of being recycled, economical efficiency and environmental protection are achieved, operation is easy, the method is suitable for industrial production, and the quality of the obtained product is superior to that of the product based on Pharmacopeia 2010.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and relates to a preparation method for synthesizing tilmicosin by using tylosin tartrate. Background technique [0002] Tilmicosin (C 46 h 80 N 2 o 13 ), the chemical name is 4A-O-de(2,6-dideoxy-3-C-methyl-L-ribose-pyranylhexyl)-20-deoxy-20-(3,5-dimethyl-1 -piperidinyl)-[20(cis:trans)]tylosin. The antibacterial spectrum of tilmicosin is similar to that of tylosin, but it has enhanced effects against Pasteurella multocida and Pasteurella hemolytica. It was successfully developed in the 1980s. The commonly used trade names are Pulmotil? and Micotil?, and the preparations include tilmicosin soluble powder, premix (20%), and injection. It was approved in most European countries in 1990, approved in the United States in 1992, and included in the United States Pharmacopoeia. Due to its special antibacterial activity and pharmacokinetic characteristics, the drug has been approved for clinical ...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/00C07H1/06
Inventor 张燕王兴路
Owner HEZE CITY FANGMING PHARMA
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