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Preparation method of high-purity fudosteine

A fudosteine, high-purity technology, applied in the field of chemical preparation, can solve the problems of difficult storage, unstable quality, difficult large-scale production, etc., and achieve the effect of stable improvement in quality and yield

Active Publication Date: 2015-03-18
TOPFOND PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The problems in the above-mentioned methods are: 1. The raw materials are not easy to obtain, the quality is unstable, difficult to store and the price is high; 2. Illumination and column chromatography generally require high process equipment conditions, and it is difficult to realize large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 169g (1M) of 48% hydrobromic acid to the 500ml cyclohexane solution of 76g (1M) of 1,3-propanediol, add 2.1gKBr, heat and reflux for 18 hours, and separate the generated water with a water separator. After the reaction was completed, the temperature was lowered to room temperature, and the cyclohexane layer was separated for further processing. The lower layer of the reaction solution was adjusted to pH = 7 with saturated sodium carbonate solution, and distilled under reduced pressure to collect 114 g of fractions with a refractive index of 1.48-1.49 (GC99.5%), with a yield of 150%.

Embodiment 2

[0024] Add 253g (1.5M) of 48% hydrobromic acid to the 750ml cyclohexane solution of 76g (1M) of 1,3-propanediol, add 2.1gKBr, heat and reflux for 18 hours, and separate the generated water with a water separator. After the reaction was completed, the temperature was lowered to room temperature, and the cyclohexane layer was separated for further processing. The lower layer of the reaction solution was adjusted to pH = 7 with saturated sodium carbonate solution, and distilled under reduced pressure to collect 121.6 g of fractions with a refractive index of 1.48-1.49 (GC99.1%), with a yield of 160%.

Embodiment 3

[0026] Add 186g (1.1M) of 48% hydrobromic acid to the 600ml cyclohexane solution of 76g (1M) of 1,3-propanediol, add 2.1gKBr, heat and reflux for 18 hours, and separate the generated water with a water separator. After the reaction was completed, the temperature was lowered to room temperature, and the cyclohexane layer was separated for further processing. The lower layer of the reaction solution was adjusted to pH = 7 with saturated sodium carbonate solution, and distilled under reduced pressure to collect 117.8 g of fractions with a refractive index of 1.48-1.49 (GC99.2%), with a yield of 155%.

[0027] B: Preparation of crude fudosteine

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Abstract

The invention provides a preparation method of a novel antitussive phlegm-eliminating drug high-purity fudosteine, wherein the preparation method includes the steps: (1) synthesizing an intermediate 3-bromo-1-propanol; (2) carrying out a reaction of cysteine hydrochloride with 3-bromo-1-propanol to obtain a crude product; and (3) carrying out crystallization refining on the obtained crude product to obtain the high-purity fudosteine. The domestic cheap easily-available raw materials of cysteine hydrochloride, hydrobromic acid and 1,3-propylene glycol materials are utilized, monitoring of a gas chromatograph, a liquid chromatograph and a refractometer is used for tracking a catalytic reaction process and a reaction terminal point. The preparation method has the advantages of less reaction steps, high selectivity, low pollution, low cost and stable quality, and is suitable for industrialized production.

Description

technical field [0001] The present invention relates to the preparation of chemicals, in particular to the preparation of high-purity fudosteine. Background technique [0002] Fudosteine ​​is a cysteine ​​derivative, which has the functions of 1) inhibiting the formation of goblet cells in airway epithelial cells; 2) normalizing the ratio of fucose and sialic acid in sputum, improving the viscosity and elasticity of sputum, and making cilia Restore the state of easy transport of airway secretions; 3) hypersecretion of serous fluid; 4) anti-inflammatory effect. [0003] Documents and disclosed patent routes have: 1) L-cysteine ​​and 3-bromopropanol thioalkylation reaction (referring to EP346883 (1989), EP5047428 (1991); 2) L-cysteine ​​and allyl alcohol add Formation reaction (referring to JP8119932, CN1840524A (2006). [0004] The problems in the above-mentioned methods are: 1. The raw materials are not easy to obtain, the quality is unstable, difficult to store and the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/58C07C319/14
Inventor 周新建
Owner TOPFOND PHARMA CO LTD
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