Preparation method of miglitol

A miglitol and reaction technology, applied in the field of miglitol preparation, can solve the problems of complicated operation, low product yield and purity, and achieve the effects of simple operation steps, high product purity and mild reaction conditions

Active Publication Date: 2020-12-29
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] Aiming at the problems of cumbersome operation, low product yield and low purity in the current preparation process of miglitol, the present invention aims to provide a simple and efficient preparation method of miglitol

Method used

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  • Preparation method of miglitol
  • Preparation method of miglitol

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Experimental program
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Effect test

Embodiment 1

[0032] In the autoclave, SM-1 (10.00g, 44.80mmol), Pd / C (0.5g), and acetic acid (5.38g, 89.6mmol) were added to the tetrahydrofuran / purified water system (V: 四氢呋喃 :V: 纯化水 =1:2, 500mL), stirring, temperature control 35 ~ 40 ° C, pressure control at 6 ± 0.5Mpa reaction 6h, the reaction is completed, the reaction solution is cooled to room temperature, and the solid concentrated under reduced pressure is filtered. The obtained solid was dissolved completely by adding ethanol (50 mL), and crystallized by adding toluene (100 mL). After the crystallization was completed, it was filtered and dried under reduced pressure to obtain miglitol with a yield of 97.5% and a purity of 99.87%.

Embodiment 2

[0034] In the autoclave, SM-1 (10.00g, 44.80mmol), Pd / C (0.8g), and acetic acid (5.92g, 98.56mmol) were added to the tetrahydrofuran / purified water system (V: 四氢呋喃 :V: 纯化水 =1:2, 500mL), stirring, temperature control 35 ~ 40 ° C, pressure control at 6 ± 0.5Mpa reaction 6h, the reaction is completed, the reaction solution is cooled to room temperature, and the solid concentrated under reduced pressure is filtered. The obtained solid was dissolved completely by adding ethanol (50 mL), and crystallized by adding toluene (100 mL). After the crystallization was completed, it was filtered and dried under reduced pressure to obtain miglitol with a yield of 95.6% and a purity of 99.97%.

Embodiment 3

[0036] In the autoclave, SM-1 (10.00g, 44.80mmol), Pd / C (0.2g), and acetic acid (4.84g, 80.60mmol) were added to the tetrahydrofuran / purified water system (V: 四氢呋喃 :V: 纯化水 =1:2, 500mL), stirring, temperature control 35 ~ 40 ° C, pressure control at 6 ± 0.5Mpa reaction 6h, the reaction is completed, the reaction solution is cooled to room temperature, and the solid concentrated under reduced pressure is filtered. The obtained solid was dissolved completely by adding ethanol (50 mL), and crystallized by adding toluene (100 mL). After the crystallization was completed, it was filtered and dried under reduced pressure to obtain miglitol with a yield of 95.5% and a purity of 99.85%.

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Abstract

The invention belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of miglitol. The method comprises the following steps: (1) adding Pd / C and SM-1 into a reaction solvent in a high-pressure reaction kettle, adding an acid, conducting stirring, controlling the temperature and pressure, carrying out hydrogenation reaction, cooling the reaction solution to room temperature after the reaction is finished, conducting filtering, and carrying out reduced pressure concentration until the reaction solution is dry to obtain a solid; and (2) adding an organic solvent into the obtained solid for dissolution, adding a crystallization solvent for crystallization, completely conducting crystallizing, conducting filtering, and carrying out vacuum drying toobtain a target compound miglitol. Compared with the prior art, the invention provides a simple, convenient and efficient method for preparing miglitol, and the whole synthesis method has the advantages of short route, simple operation steps, high reaction yield, high product purity, mild reaction conditions, effective shortening of the production period, and suitableness for industrial scale-upproduction.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a preparation method of miglitol. Background technique [0002] Miglitol, chemical name: (2R,3R,4R,5S)-2-hydroxymethyl-1-(2-hydroxyethyl)-3,4,5,-piperidinetriol, white or Off-white powder is a new type of hypoglycemic drug researched and developed by German Bayer Pharmaceutical Company in the early 1980s. Its chemical structural formula is as follows: [0003] [0004] The pathogenesis of type II diabetes is closely related to genetic and environmental factors, among which genetic factors include insulin resistance or deficiency, obesity and intrauterine growth retardation, etc., while acquired obesity, sedentary, smoking and exogenous toxins belong to the environment factor. The function of islets in patients is not completely lost, and some patients even have hyperfunction of islets, but lack of insulin that really exerts the hypoglycemic effect. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/46
CPCC07D211/46Y02P20/55
Inventor 张贵民陈迎会张清德
Owner LUNAN PHARMA GROUP CORPORATION
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