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Method for preparing xanthydrol from xanthones as raw material

A technology of xanthone and xanthanol, which is applied in the field of solvents used in the preparation process, can solve the problems of low solvent recovery rate, industrial production limitation, and high consumption of reducing agent, etc., and achieve the prospect of large-scale industrialization and facilitate industrialization The effect of shortening production and reaction time

Inactive Publication Date: 2008-12-24
上海五洲同一药业有限公司
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Problems solved by technology

[0003] At present, when using said xanthenone as a raw material to prepare xanthanol, zinc powder is usually used as a reducing agent and formaldehyde ester is used as a solvent for preparation. This reaction has significant defects, such as long reaction time and low yield. , the consumption of reducing agent is high, and the recovery rate of solvent is not high, so the industrial production is limited

Method used

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  • Method for preparing xanthydrol from xanthones as raw material

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Effect test

Embodiment 1

[0014] 60 kg of xanthone in 125 kg of toluene, and 30 kg of zinc powder are subjected to a reduction reaction in the presence of a theoretical amount of sodium hydroxide, the reaction temperature is 105 ° C, and the reaction time is 17 hours to obtain xanthanol, which is then heated and recovered Solvent, enter the next reaction process, you can get 42.00 kg of zhan ton acid, the yield is 60.71%.

Embodiment 2

[0016] 60 kilograms of xanthone in 125 kilograms of toluene, and 32 kilograms of zinc powders are subjected to a reduction reaction in the presence of a theoretical amount of sodium hydroxide, the reaction temperature is 112 ° C, and the reaction time is 15 hours to obtain xanthanol, which is then heated and recovered Solvent, enter the next reaction process, you can get 42.01 kg of zhan ton acid, the yield is 60.72%.

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Abstract

The invention provides a method for preparing xanthene ethanol by taking xanthene ketone as a raw material, comprising the following steps that: the xanthene ketone and zinc powder have reduction reaction in a solvent in the presence of alkali metal hydroxide, the solvent is toluene and a target product is collected from the reaction product. In the method, the zinc powder consumption amount is reduced evidently and is only 80 percent of that of the prior art, and the production cost is lowered greatly; and the toluene is taken as the solvent and is easy to reclaim, and the cost is greatly lower than formaldehyde ester, the reaction time is shortened, the reaction yield is improved, the industrial production is convenient, and the method has great industrialized implementation prospect.

Description

technical field [0001] The invention relates to a method for preparing xanthanol by using xanthenone as a raw material, in particular to a solvent used in the preparation process. Background technique [0002] Xanthenic acid is an intermediate for preparing propantheline bromide. At present, the conventional method is to use xanthone as a raw material, using a reducing agent, and performing a reduction reaction in a solvent to generate xanthene alcohol, followed by cyanation and hydrolysis. Prepared. The chemical name of Xanthene-9-carboxylic acid is Xanthene-9-carboxylic acid, and its molecular formula is: C 14 h 10 o 3 . [0003] At present, when using said xanthenone as a raw material to prepare xanthanol, zinc powder is usually used as a reducing agent and formaldehyde ester is used as a solvent for preparation. This reaction has significant defects, such as long reaction time and low yield. , the reducing agent consumes a lot, and the solvent recovery rate is not h...

Claims

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Application Information

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IPC IPC(8): C07D311/86
Inventor 冯桂春
Owner 上海五洲同一药业有限公司
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