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Method for separating all trans-teprenone under low temperature

A technology of teprenone and all-trans, applied in the field of separating all-trans teprenone at low temperature, achieving controllable separation temperature, solving separation problems, and high content

Inactive Publication Date: 2017-02-22
TIANJIN RUIAN MEDICAL TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] As a novel gastric mucosal protective agent, teprenone has a good therapeutic effect on acute and chronic gastritis and gastric ulcer, but at the present stage the pharmaceutical industry uses cis-trans isomers (cis:trans=2:3 ), and a variety of data show that only the trans-teprenone is the main active ingredient, and the cis- and trans-forms are difficult to separate by high-temperature distillation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A method for separating all-trans teprenone at low temperature, the specific steps are:

[0017] (1) Preparation of diluent: add tetrahydrofuran to low-chain liquid alkane, the mass-to-number ratio of the two is 100:1, stir well and evenly, and configure it as a diluent;

[0018] (2) Add the prepared diluent into a jacketed container, then add the teprenone mixture, the mass-number ratio of the mixture of diluent and teprenone is 100:10, start stirring, and Put circulating hot water into the jacket, control the temperature in the container to 0°C, stir thoroughly for 1 hour, and control the stirring speed to 60r / min to make it fully mixed;

[0019] (3) Discharge the circulating hot water in the jacket of the container, then feed the refrigerant, control the temperature of the refrigerant, and reduce the solution temperature to -10°C, control the stirring speed to 10r / min, and keep it warm for 1 hour; then continue to cool down to reduce the solution temperature Cool do...

Embodiment 2

[0025] A method for separating all-trans teprenone at low temperature, the specific steps are:

[0026] (1) Preparation of diluent: add tetrahydrofuran to low-chain liquid alkanes, the mass-to-number ratio of the two is 100:100, fully stir evenly, and configure as diluent;

[0027] (2) Add the prepared diluent into a jacketed container, then add the teprenone mixture, the mass-number ratio of the mixture of diluent and teprenone is 100:150, start stirring, and Put circulating hot water into the jacket, control the temperature in the container to 60°C, stir thoroughly for 3 hours, and control the stirring speed to 180r / min to make it fully mixed;

[0028] (3) Discharge the circulating hot water in the jacket of the container, then feed the refrigerant, control the temperature of the refrigerant, and reduce the solution temperature to -30°C, control the stirring speed to 50r / min, and keep the heat for 5 hours; then continue to cool down, and the solution temperature Decrease to...

Embodiment 3

[0034] A method for separating all-trans teprenone at low temperature, the specific steps are:

[0035] (1) Preparation of diluent: add ethyl propyl ether to low-chain liquid alkanes, the mass-to-number ratio of the two is 100:50, stir well and evenly, and configure diluent;

[0036] (2) Add the prepared diluent into a jacketed container, then add the teprenone mixture, the mass-number ratio of the mixture of diluent and teprenone is 100:80, start stirring, and Put circulating hot water into the jacket, control the temperature in the container to 30°C, stir fully for 2 hours, and control the stirring speed to 120r / min to make it fully mixed;

[0037] (3) Discharge the circulating hot water in the jacket of the container, then feed the refrigerant, control the temperature of the refrigerant, and reduce the solution temperature to -25°C, control the stirring speed to 30r / min, and keep it warm for 3 hours; then continue to cool down to reduce the solution temperature Cool down t...

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PUM

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Abstract

The invention relates to a method for separating all trans-teprenone under low temperature. The method comprises the following specific steps: an ether-type organic solvent is added in low-chain liquid alkane, and full and uniform stirring is performed, such that a diluting agent is prepared; the prepared diluting agent is added into a jacketed container; a teprenone isomer mixture is added; stirring is started; circulating hot water is introduced into the jacket; stirring is carried out for uniformly mixing the materials; the circulating hot water in the container jacket is discharged, and a refrigerant is introduced; crystallization is carried out under stirring, such that teprenone crystals are obtained; the teprenone crystals are placed in a vacuum suction filtration device, and vacuum suction filtration is carried out; an upper-layer filter cake is taken out and is dissolved under normal temperature, such that all trans-teprenone is obtained. The method assists in fundamentally solving an all trans-teprenone separation problem. The separation temperature is controllable. The all trans-teprenone obtained after separation has the advantages of high content and low impurity content. During the process, solvent amount is low; the solvent can be recycled and applied mechanically; and no three-waste is generated. The method is suitable for large-scale production.

Description

technical field [0001] The invention relates to the fields of chemical synthesis and pharmacy, in particular to a method for separating all-trans teprenone at low temperature. Background technique [0002] As a novel gastric mucosal protective agent, teprenone has a good therapeutic effect on acute and chronic gastritis and gastric ulcer, but at the present stage the pharmaceutical industry uses cis-trans isomers (cis:trans=2:3 ), and a variety of data show that only the trans-teprenone is the main active ingredient, and the cis- and trans-forms are difficult to separate by high-temperature distillation. Contents of the invention [0003] The invention aims to solve the deficiencies of the prior art, and provides a method for separating all-trans teprenone at low temperature. [0004] In order to achieve the above object, the present invention adopts the following technical solutions: [0005] A method for separating all-trans teprenone at low temperature, the specific s...

Claims

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Application Information

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IPC IPC(8): C07C45/81C07C49/203
CPCC07C45/81C07B2200/09C07C49/203
Inventor 杜勇雄张玮杨慧敏王玉龙刘鹏刘宝峰杜躺雄
Owner TIANJIN RUIAN MEDICAL TECH DEV
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