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Purification method of alpha-tropine

A purification method and tropine technology, applied in the direction of organic chemistry, etc., can solve the problems of high toxicity of solvent acetone, etc., and achieve the effect of reducing environmental damage

Active Publication Date: 2013-05-01
SHANGQIUSOHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the α-Tropine alcohol crystal purity that the present invention obtains is higher, the toxicity of solvent acetone is bigger, is easy poisonous solvent again

Method used

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  • Purification method of alpha-tropine

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Effect test

Embodiment 1

[0009] A kind of purification method of α-tropine alcohol, after the ethanol solution 30g containing α-tropine alcohol is distilled off under reduced pressure to remove ethanol, obtain solid crystal 10g, add 20g ethyl acetate and 1g gac, heat under the condition of 60 ℃ After 0.5 hours, filter, place the filtrate to crystallize, and crystallize at 0° C. for 5 hours. After filtering, wash the crystals with ethyl acetate, and dry them in vacuum at 40° C. to obtain α-tropine alcohol crystals.

Embodiment 2

[0011] A kind of purification method of α-tropine alcohol, after the ethanol solution 30g containing α-tropine alcohol is distilled off under reduced pressure to remove ethanol, obtain solid crystallization 10g, add 60g ethyl acetate and 0.6g gac, under the condition of 70 ℃ Heat to reflux for 1 hour, filter, place the filtrate to crystallize, crystallize at -5°C for 2 hours, filter, wash the crystals with ethyl acetate, and dry in vacuum at 50°C to obtain α-tropine alcohol crystals.

Embodiment 3

[0013] 1. a kind of purification method of α-tropine alcohol, after the ethanol solution 30g decompression distillation that will contain α-tropine alcohol removes ethanol, obtain solid crystal 10g, add 40g ethyl acetate and 1.2g gac, at 65 ℃ Heating under the conditions for 0.5 hours, filtering, leaving the filtrate to crystallize, and crystallizing at -2°C for 3 hours, filtering, washing the crystals with ethyl acetate, and drying in vacuum at 60°C to obtain α-tropine alcohol crystals.

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Abstract

The invention discloses a purification method of alpha-tropine. The purification method comprises the following steps of: distilling an ethanol solution containing alpha-tropine under reduced pressure for removing ethanol so as to obtain solid crystals; adding ethyl acetate and activated carbon in the solid crystals, and heating and refluxing for 0.5-1 hour at the temperature of 60-80 DEG C; filtering, and standing a filtrate for crystallization; crystallizing for 1-5 hours at the temperature of minus10 DEG C-5 DEG C; and filtering, crystallizing, washing with ethyl acetate, and drying at a vacuum condition at the temperature of 40-60 DEG C so as to obtain the alpha-tropine crystals. By high performance gas chromatography analysis, the purity of alpha-tropine is more than 99%, the yield of alpha-tropine is more than 80%; and the used solvent ethyl acetate is an environmentally-friendly solvent, thereby reducing the damage on environment.

Description

technical field [0001] The invention relates to a method for purifying alpha-tropine alcohol. Background technique [0002] Atropine is a parasympathetic depressant and can be used as a mydriatic and laxative in ophthalmology. At present, in the production process of atropine, α-tropine alcohol is put into the next step reaction in liquid form. If impurities containing β-tropine alcohol are put into the next step reaction and participate in the reaction, not only the final product atropine The quality of the reaction is greatly affected, which complicates the post-treatment and reduces the yield of the reaction. Chinese patent 200910153662.1 discloses a method for purifying tropinol in the atropine production process. The ethanol solution containing α-tropineol is distilled under reduced pressure to recover ethanol, and solid crystals are obtained, then acetone is added, and the temperature is lowered to 5-15°C. After crystallization for 1.5 to 2 hours, filter to obtain pu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D451/06
Inventor 孙韶军孙随军肖红燕
Owner SHANGQIUSOHUA PHARMA
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