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Preparing technology of beta-D-galactosamine pentaacetate

The technology of pentaacetate and galactosamine is applied in the field of preparation technology of β-D-galactosamine pentaacetate, can solve the problems of complicated synthesis process, low purity and high cost, and achieves simple synthesis steps, The effect of high purity and simple process

Inactive Publication Date: 2019-08-23
南京博源医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] β-D-galactosamine pentaacetate is a relatively common pharmaceutical intermediate, which is used in pharmaceutical synthesis. The existing synthesis process of β-D-galactosamine pentaacetate is cumbersome, with high cost and low purity. , D-galactose is a component of agar, plant gum, viscose and raffinose, lactose, melibiose and other sugars

Method used

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  • Preparing technology of beta-D-galactosamine pentaacetate

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Effect test

Embodiment 1

[0020] The preparation technology of a kind of β-D-galactosamine pentaacetate that the present invention proposes, comprises the following steps,

[0021] S1, D-galactose and vinyl acetate are used as raw materials, anhydrous sodium acetate is used as a catalyst, and a mixed solvent of toluene and benzene is used as a reaction solvent. The raw materials and reaction solvent are placed in a reaction kettle, and the reaction temperature is controlled at 40°C. The reaction time was 15 minutes, distilled under reduced pressure, filtered, recovered the filtrate, washed the filtrate with ethanol, and vacuum-dried to constant weight to obtain β-D-galactose pentaacetate;

[0022] S2, put the β-D-galactose pentaacetate obtained in S1 into the reaction kettle, then add thioacetamide, then add an organic solvent, control the temperature at 22°C, react for 45min, stop heating, and obtain a mixed solution A;

[0023] S3, the mixed solution A is extracted with an extraction solvent, washed...

Embodiment 2

[0025] The preparation technology of a kind of β-D-galactosamine pentaacetate that the present invention proposes, comprises the following steps,

[0026] S1, D-galactose and vinyl acetate are used as raw materials, anhydrous sodium acetate is used as a catalyst, and a mixed solvent of toluene and benzene is used as a reaction solvent. The raw materials and reaction solvent are placed in a reaction kettle, and the reaction temperature is controlled at 50°C. The reaction time is 20 minutes, distilled under reduced pressure, filtered, recovered the filtrate, washed the filtrate with ethanol, and dried in vacuum to constant weight to obtain β-D-galactose pentaacetate;

[0027] S2, put the β-D-galactose pentaacetate obtained in S1 into the reaction kettle, then add thioacetamide, then add an organic solvent, control the temperature at 25°C, react for 55min, stop heating, and obtain a mixed solution A;

[0028] S3, the mixed solution A is extracted with an extraction solvent, wash...

Embodiment 3

[0030] The preparation technology of a kind of β-D-galactosamine pentaacetate that the present invention proposes, comprises the following steps,

[0031] S1, D-galactose and vinyl acetate are used as raw materials, anhydrous sodium acetate is used as a catalyst, and a mixed solvent of toluene and benzene is used as a reaction solvent. The raw materials and the reaction solvent are placed in a reaction kettle, and the reaction temperature is controlled at 55°C. The reaction time was 35 minutes, distilled under reduced pressure, filtered, recovered the filtrate, washed the filtrate with ethanol, and vacuum-dried to constant weight to obtain β-D-galactose pentaacetate;

[0032] S2, put the β-D-galactose pentaacetate obtained in S1 into the reaction kettle, then add thioacetamide, then add an organic solvent, control the temperature at 28°C, react for 75min, stop heating, and obtain a mixed solution A;

[0033] S3, the mixed solution A is extracted with an extraction solvent, wa...

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Abstract

The invention discloses a preparing technology of beta-D-galactosamine pentaacetate, and belongs to the field of medical intermediates. The preparing technology comprises the following steps of S1, taking D-galactose and vinyl acetate as raw materials, taking sodium acetate anhydrous as a catalyst, taking a mixed solvent of methylbenzene and benzene as a reaction solvent, putting the raw materialsand the reaction solvent into a reaction kettle, conducting reduced pressure distillation and filtering, recycling a filtrate, utilizing ethyl alcohol for washing the filtrate, and conducting vacuumdrying to constant weight to obtain the beta-D-galactosamine pentaacetate; S2, putting the beta-D-galactosamine pentaacetate obtained in S1 into the reaction kettle, then putting thioacetamide, then adding an organic solvent, controlling the temperature to be 22-28 DEG C, carrying out a reaction for 45-75 min, and stopping heating to obtain a mixed solution A. The preparing technology is simple and reasonable, the synthesis steps are simple, the purity of the beta-D-galactosamine pentaacetate obtained through crystallization is high, large-scale production can be achieved, and the preparing technology is suitable for application and popularization.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical intermediates, in particular to a preparation process of β-D-galactosamine pentaacetate. Background technique [0002] The so-called pharmaceutical intermediates are actually some chemical raw materials or chemical products used in the process of pharmaceutical synthesis. This kind of chemical product does not require a drug production license, and can be produced in ordinary chemical factories. As long as it reaches a certain level, it can be used in the synthesis of drugs. [0003] β-D-galactosamine pentaacetate is a relatively common pharmaceutical intermediate, which is used in pharmaceutical synthesis. The existing synthesis process of β-D-galactosamine pentaacetate is cumbersome, with high cost and low purity. , D-galactose is a component of agar, plant gum, viscose and raffinose, lactose, melibiose and other sugars. Exist in snail protein glands, frog eggs, brain nerve tissue and o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/12C07H1/00
CPCC07H1/00C07H15/12
Inventor 陈建国袁新辉
Owner 南京博源医药科技有限公司
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