Production technique of fudosteine

A production process, fudosteine ​​technology, applied in the field of fudosteine ​​production process, can solve the problems of low product purity and low yield, and achieve the effects of reducing occupational hazards, low cost, and mild reaction conditions

Inactive Publication Date: 2016-06-01
ANHUI YOUCARE KAIYUE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many types of synthetic techniques for fudosteine ​​in the prior art, but most of them have defects such as low yield and low product purity.

Method used

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  • Production technique of fudosteine
  • Production technique of fudosteine
  • Production technique of fudosteine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0017] 1. Production raw materials:

[0018] raw material name

Production usage

Specification

purpose

L-cysteine

15.2kg

CP

starting material

Acryl alcohol

14kg

CP

Reactive ingredients

Potassium persulfate

1.5kg

AR

catalyst

Absolute ethanol

114kg

CP

Reaction solvent

activated carbon

0.190kg

Medicinal

bleaching

[0019] 2. Production process

[0020] (1) synthesis of fudosteine ​​crude product

[0021] Feeding

[0022]

[0023]

[0024] Theoretical output value: Fudosteine ​​crude product 18.8Kg

[0025] Specific operation process:

[0026] In a 500L glass-lined reactor, dissolve 15.2kg of L-cysteine ​​in 140.0kg of purified water, stir and dissolve, add 1.5kg of potassium persulfate and 14kg of propylene alcohol, after the addition is complete, stir and react at a temperature of 30±2°C for 5 After ±1h, evaporate the solvent to dryness under redu...

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PUM

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Abstract

The invention relates to a production technique of fudosteine. The production technique comprises the following steps: dissolving L-cysteine in purified water by stirring, adding potassium persulfate and propenol, and stirring to react for 5+/-1 hours while controlling the temperature at 30+/-2 DEG C; distilling under reduced pressure to remove the solvent; adding ethanol into the residues, stirring for 1.5 hours, and filtering to remove insoluble substances; concentrating the filtrate until a small amount of solid precipitates, and stopping concentrating; cooling, crystallizing by stirring at 30+/-2 DEG C for 3+/-1 hours until abundant white solid appears, and carrying out centrifugal filtration; washing the filter cake with anhydrous ethanol twice, and drying to obtain a fudosteine crude product; and refining and drying to obtain the fudosteine. By using ethanol-water as the solvent, the technique has the advantages of high use safety, low cost, mild reaction conditions and high atom economic benefit, and conforms to the requirements for green chemistry. The product yield is up to 95% or above, the content is up to 99.9%, and the maximum single impurity content is lower than 0.01%. Besides, the technique reduces the occupational hazards for employees, and is more beneficial to mass production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a production process of fudosteine. Background technique [0002] Fudosteine, white or off-white crystalline powder, odorless, slightly sweet taste, molecular formula C 6 h 13 NO 3 S, its chemical structural formula is as follows: [0003] [0004] Fudosteine ​​is an expectorant with a new mechanism of action. It can inhibit the excessive formation of mucus-secreting goblet cells in the trachea and the production of highly viscous fucoidin. It has good antitussive and phlegm-reducing effects. Efficacy, it was first approved in Japan in October 2001 to be produced and marketed by Mitsubishi Pharmaceutical Co., Ltd. and SS Pharmaceutical Co., Ltd. But for now, it still has a great market demand. There are many types of fudosteine ​​synthesis techniques in the prior art, but most of them have defects such as low yield and low product purity. Contents of the in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/58C07C319/18C07C319/28
CPCC07C319/18C07C319/28
Inventor 周如国刘维坦高彬洁
Owner ANHUI YOUCARE KAIYUE PHARMA
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