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Method for recovering guanine from centrifugal mother liquor of 2, 9-diacetyl guanine

A technology of diacetylguanine and centrifugal mother liquor, applied in the field of guanine recovery, can solve the problems of reducing the utilization rate of raw materials, a large amount of solid waste, waste of useful resources, etc., and achieve effective recycling, realization of resources, and improvement of raw material utilization rate. Effect

Inactive Publication Date: 2018-11-23
江苏八巨药业有限公司
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Problems solved by technology

But the following technical problems exist in the existing preparation process: the reaction is not complete in the preparation process, and the solvent is recovered by distillation of the supernatant after centrifugation, but part of the 2,9-diacetylguanine product is dissolved in the reaction centrifugation mother liquor (supernatant) , will generate a large amount of solid waste, reduce the utilization rate of raw materials, waste useful resources, and is not conducive to environmental protection and sustainable development of enterprises

Method used

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  • Method for recovering guanine from centrifugal mother liquor of 2, 9-diacetyl guanine
  • Method for recovering guanine from centrifugal mother liquor of 2, 9-diacetyl guanine
  • Method for recovering guanine from centrifugal mother liquor of 2, 9-diacetyl guanine

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Effect test

Embodiment 1

[0034] Put 50g of guanine, 250g of acetic anhydride, 90g of acetic acid and 0.1g of PTS into a clean and dry 500mL three-neck flask, start stirring, start heating to reflux, react for 10 hours, and centrifuge to obtain the centrifuged mother liquor. The centrifuged mother liquor is distilled and concentrated, and the bottom material is concentrated Add 200 ml of dilute hydrochloric acid with a concentration of 10% by mass, heat until dissolved, then add 3 g of activated carbon, heat up and reflux for 2 hours for hydrolysis and decolorization, filter while it is hot, cool the filtrate to 15°C, cool and crystallize, filter to obtain bird Purine hydrochloride wet product, then add guanine hydrochloride to 80 ml of sodium hydroxide solution with a concentration of 5% by mass, heat up to dissolve, add 0.4 g of activated carbon, heat up and reflux for 30 minutes for decolorization, and filter while hot , the filtrate was acidified by adding concentrated hydrochloric acid to adjust th...

Embodiment 2

[0036] Put 50g of guanine, 250g of acetic anhydride, 90g of acetic acid and 0.1g of PTS into a clean and dry 500mL three-neck flask, start stirring, start heating to reflux, react for 10 hours, and centrifuge to obtain the centrifuged mother liquor. The centrifuged mother liquor is distilled and concentrated, and the bottom material is concentrated Add 200 ml of dilute sulfuric acid with a concentration of 10% by mass, heat to dissolve, then add 3 g of activated carbon, heat up and reflux for 2.5 hours for hydrolysis and decolorization, filter while it is hot, cool the filtrate to 12 ° C, cool and crystallize, filter to obtain bird Purine sulfate wet product, then guanine hydrochloride is added to 80 ml of sodium carbonate solution with a concentration of 8% by mass, heated and dissolved, added 0.4 g of activated carbon, heated and refluxed for 30 minutes for decolorization, filtered while hot, The filtrate was acidified by adding sulfuric acid with a mass percentage concentrat...

Embodiment 3

[0038] Put 50g of guanine, 250g of acetic anhydride, 90g of acetic acid and 0.1g of PTS into a clean and dry 500mL three-neck flask, start stirring, start heating to reflux, react for 10 hours, and centrifuge to obtain the centrifuged mother liquor. The centrifuged mother liquor is distilled and concentrated, and the bottom material is concentrated Add 300 ml of hydrochloric acid with a mass percentage concentration of 12%, heat to dissolve, then add 4 g of activated carbon, heat up and reflux for 3 hours for decolorization, filter while hot, cool the filtrate to 10°C, cool and crystallize, filter to obtain guanine Sulphate wet product, then guanine hydrochloride was added to 90 milliliters of potassium hydroxide solution with a concentration of 5% by mass, heated and heated to dissolve, added 0.5 g of activated carbon, heated and refluxed for 30 minutes for decolorization, filtered while hot, The filtrate was acidified by adding concentrated hydrochloric acid to adjust the pH ...

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Abstract

In order to solve the problem of generation of large amount of solid wastes in solvent recovery from distillation of the conventional process for 2, 9-diacetyl guanine, the invention provides a methodfor recovering the guanine from centrifugal mother liquor obtained by adopting the guanine as a raw material to prepare the 2, 9-diacetyl guanine. The method comprises the following steps of: addingacid solution into the centrifugal mother liquor of the 2, 9-diacetyl guanine, separating out a certain acid salt of the guanine, adding alkali liquor into guanine hydrochloride, crystallizing and recovering to obtain the guanine. The method provided by the invention has the beneficial effects that the conventional step of preparing the 2, 9-diacetyl guanine by adopting the guanine as the raw material is improved, the raw material and products in the centrifugal mother liquor are recovered and reutilized, the purity of the recovered guanine is higher than 99%, so that the recovered guanine canreact again, the utilization ratio of the raw material can be increased, and the process is environment-friendly and economical, realizes effective circulating use of resources and is beneficial to sustainable development of enterprises.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and relates to a series of preparation methods of important intermediates of anti-herpes drugs such as acyclovir and famciclovir with high efficiency and low toxicity. A method for recovering guanine from purine centrifugal mother liquor. Background technique [0002] Chemical name: Guanine, the English name is Guanine, and the structural formula is as follows: [0003] [0004] Guanine is an important intermediate of a series of high-efficiency and low-toxic anti-herpes drugs such as acyclovir and famciclovir. In particular, acyclovir is an anti-herpes drug with high efficiency and low toxicity, which has a broad market prospect and has attracted extensive attention from various medical circles. [0005] At present, the synthesis process of 2,9-diacetylguanine generally uses guanine and acetic anhydride as raw materials, introduces acetyl groups at the 2 and 9 positio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/18
CPCC07D473/18
Inventor 程焕达楚玮明孔立程加铭张进福陈恬
Owner 江苏八巨药业有限公司
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