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Moguisteine synthesis process

A technology of synthesis process and process steps, applied in the field of medicine, achieves the effects of easy operation, simple equipment and reduced production cost

Inactive Publication Date: 2012-09-05
FOSHAN DAYI TECH LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The present invention aims at various problems existing in the present mogistein synthesis technique, and provides a kind of mogistein synthesis technique that solves the above problems

Method used

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Examples

Experimental program
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Embodiment 1

[0030] Embodiment 1, prepare mogisteine ​​according to the following processing steps:

[0031] (1) Acyl chloride synthesis reaction generates monoethyl malonate acid chloride: add 26.42 g (0.2 mol) of monoethyl malonate in a 500 ml flask, add 100 ml of dichloromethane, stir in an ice bath for 10 minutes, and drop from the dropping funnel Add 17ml (0.24mol) of thionyl chloride, after the dropwise addition, continue to stir for 10 minutes, then heat and reflux for 1 hour, then cool and stir in an ice bath for 10 minutes, add 100ml of water, stir, and separate the liquids to obtain light brown malonic acid Dichloromethane solution of monoethyl chloride;

[0032] (2) preparation of dichloromethane solution of monoethyl malonate acid chloride

[0033] Add 34.05 g (0.2 mol) of potassium monoethyl malonate to a 500 ml flask, add 100 ml of dichloromethane, stir in an ice bath for 10 minutes, add 17 ml (0.24 mol) of thionyl chloride dropwise from the dropping funnel, and the addition...

Embodiment 2

[0037] Embodiment 2, by the operation method of step 4 in embodiment 1, use the dichloromethane solution of the malonate monoethyl chloride prepared in step 2 in embodiment 1, obtain mogistein white powder 27.8g, yield is according to Guaifenesin 82%. The melting point is 73.2-74.5°C.

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Abstract

The invention relates to the technical field of medicines, in particular to a moguisteine synthesis process. The moguisteine synthesis process provided by the invention comprises the following steps of: generating ethyl malonyl chloride by adopting acyl chloride synthesis reaction; layering and then acquiring an organic layer containing a dichloromethane solution of acyl chloride as a dichloromethane solution of acyl chloride; and dropping the dichloromethane solution of the acyl chloride of the organic layer into a dichloromethane solution of (+ / -)-2-((2-methoxyphenoxy)methyl) thiazolidine for reacting to obtain moguisteine. The moguisteine synthesis operation is simplified, the equipment is simple, the operation is easy, the prepared moguisteine has higher purity, and the production cost of the moguisteine is lowered.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a mogistein synthesis process. Background technique [0002] Coughing is an important reflex protection mechanism. Coughing can expel sputum and foreign objects in the respiratory tract, protect the cleanliness and smoothness of the respiratory tract, and prevent infection. However, if the severe cough persists, not only the patient suffers, but also other complications are likely to occur. With the aggravation of social environmental pollution and the increasing incidence of respiratory diseases, expectorant and antitussive drugs will be an important part of respiratory system drugs, so it is necessary to choose appropriate antitussives to relieve cough. [0003] Mogisteine ​​((+ / -)-2-((2-methoxyphenoxy)methyl)-3-ethoxycarbonylacetyl-1,3-thiazolidine) is an acetylcholine antagonist , the structural formula is as shown in formula III: [0004] [0005] Formula III [0006...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/04
Inventor 唐良伟雍智全闻亚磊阴元魁雷安胜伍伟成
Owner FOSHAN DAYI TECH LTD
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