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Preparation method of D-panthenol

A refining method and panthenol technology, applied in the field of preparation of high optical purity D-panthenol, can solve the problems of low optical rotation value, unsatisfactory, and incomplete removal of reaction solvent ethanol, etc., so as to improve quality, obtain raw materials easily, reduce Costs and Effects of Environmental Pollution

Active Publication Date: 2010-10-06
北京藏卫信康医药研发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The synthetic method of D-panthenol is reported in Modern Chemicals (26), 2006, 186-188 respectively, and its preparation technology is that D-(-)-pantoate lactone and 3-amino-1-propanol are prepared in ethanol. Under the condition of solvent, after heating and reacting, D-panthenol is obtained by concentration under reduced pressure. This process reaction requires ethanol as a solvent. Since D-panthenol is a viscous liquid, concentration under reduced pressure often cannot completely remove the reaction solvent ethanol. At the same time, the product The color is yellow, and the optical rotation value is low. None of the above can meet the requirements of pharmaceutical D-panthenol, especially the injection containing D-panthenol, which requires higher quality requirements such as purity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take 1.0kg of D-(-)-pantolactone and 580g of 3-amino-1-propanol into the reactor, heat to 50°C, react for 3 hours, and cool down to room temperature to obtain the D-panthenol product, clear Viscous liquid that is easy to absorb moisture, 1.58kg of finished product is obtained, and the product yield is 100%. The product is inspected by the above-mentioned quality control method, and all quality control indicators are in compliance with the regulations, and the specific rotation is +30.0°.

Embodiment 2

[0037]Weigh 3kg of D-(-)-pantolactone and add to a 10L heating reactor; measure 6L of ethyl acetate and add to the reactor, heat and stir, add 5g of activated carbon after reflux, and decolorize for 30 minutes; suction filter, Put the filtrate into a 25L container, add 12L of petroleum ether, mix well, and then stand for crystallization at 5°C for 2h; suction filter the solid, then dry the solid under vacuum at 40°C for 2h, and recover the filtrate; add 5L of ethyl acetate to the solid, and heat to reflux under stirring , add 5g of activated carbon, decolorize for 30 minutes; filter, add the filtrate into a 25L container, add 10L of petroleum ether, mix and stand for crystallization at 5°C for 2h; suction filter, and then vacuum dry the solid at 40°C for 10 hours to obtain 2.7kg of white solid Yield 90%. Take 1.0kg of refined D-(-)-pantolactone and 580g of 3-amino-1-propanol into the reactor, heat to 50°C, react for 3 hours, and cool down to room temperature to obtain D-panthe...

Embodiment 3

[0039] Weigh 3kg of D-(-)-pantolactone and add it to a 10L heating reactor; measure 6L of acetone and add it to the reactor, heat and stir, add 5g of activated carbon after reflux, and decolorize for 30 minutes; filter with suction and add the filtrate Into a 25L container, add 12L of petroleum ether, mix well, and then stand for crystallization at 5°C for 2h; filter the solid, then dry it in vacuum at 40°C for 2h; add 5L of acetone to the solid, heat to reflux under stirring, add 5g of activated carbon, and decolorize for 30 Minutes; filter, add the filtrate to a 25L container, add 10L of petroleum ether, mix and stand for crystallization at 5°C for 2h; filter with suction, then dry the solid under vacuum at 40°C for 10 hours to obtain 2.6kg of white solid, with a yield of 87%. Take 1.0kg of refined D-(-)-pantolactone and 580g of 3-amino-1-propanol into the reactor, heat to 60°C, and react for 3h. The D-panthenol product is obtained when it is lowered to room temperature. It ...

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Abstract

The invention relates to a preparation method of D-panthenol. D-(-)-pantolactone is reacted with 3-amino-1-propanol in the absence of solvent to obtain the high-purity D-panthenol, and the overall yield is more than 80%.

Description

technical field [0001] The invention relates to a preparation method of D-panthenol, in particular to a preparation method of D-panthenol with high optical purity. Background technique [0002] Panthenol commonly known as provitamin B 5 , Ubiquinol can be divided into three forms: DL-type, D-type and L-type, of which only the D-type has biological activity, and the L-type has no biological activity. D-panthenol, also known as dexpanthenol, is an optically active stereoisomer of panthenol, and its English name is dexpanthenol; D-pantothenyl aleohol. [0003] Dexpanthenol (D-panthenol) is the equivalent of D-pantothenic acid, the precursor of coenzyme A, and an important vitamin drug. It can be converted into pantothenic acid in the human body and then synthesized into coenzyme A, which promotes human protein, fat, and sugar. Metabolism of class, protect the mucous membrane and luster of the skin surface, and prevent the occurrence of diseases. Hair lotion, mousse, moisturi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C235/08C07C231/02
Inventor 曹志华胡军刘烽张勇
Owner 北京藏卫信康医药研发有限公司
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