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Preparation method of xanthine

A technology of xanthine and guanine, which is applied in the field of preparation of purine drug intermediates, can solve the problems of cumbersome production process steps, difficult waste treatment, high safety risk, etc., and achieve suppression of side reactions, high molar yield, and high product purity Effect

Active Publication Date: 2019-01-25
潍坊奥通药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] In view of the defects in the existing production technology such as large amount of three wastes, difficult waste treatment, high safety risk and cumbersome production process steps, the present invention provides a production of three wastes with low production volume, easy treatment and recycling, and simple process steps. Preparation method of xanthine with high yield and purity

Method used

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  • Preparation method of xanthine
  • Preparation method of xanthine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] 200g of purified water, 66g of 33% concentrated hydrochloric acid, and 30g of guanine (0.1985mol) were sequentially put into a 500mL three-necked flask, stirred, heated to 85°C and stirred for 0.5h. Then, 50 g of 40% sodium nitrite aqueous solution (0.2899 mol) was slowly added dropwise at 20°C.

[0054] After dropping, raise the temperature to 45°C to continue the reaction for 2 hours, cool down to 15°C, press filter, wash, and the filtrate can be applied to the next batch of "diazotization" feeding. 56 g of AH01 were obtained.

[0055] Put 250g of purified water and 56g of AH01 into a 500mL enamel reaction kettle, start stirring, and heat up to 80°C for 2.0 hours of hydrolysis reaction. After the reaction was completed, 65 g of 27% ammonia water (0.5007 mol) was added. Heat up to 80°C to dissolve, add 2g of activated carbon to decolorize for 0.5h, press filter while hot, and cool the filtrate to 25°C to grow crystals for 1h. Suction filter to dryness, wash the filt...

Embodiment 2

[0058] Put 250g of the above batch of AH01 filtrate, 25g of 33% concentrated hydrochloric acid, and 30g of guanine (0.1985mol) into a 500mL flask in turn, stir, and raise the temperature to 85°C to stir for 0.5h. Then, 40 g of 40% sodium nitrite aqueous solution (0.2319 mol) was slowly added dropwise at 20°C.

[0059] After dropping, raise the temperature to 45°C to continue the reaction for 2 hours, cool down to 15°C, press filter, wash, and the filtrate can be applied to the next batch of "diazotization" feeding. 57 g of AH01 were obtained.

[0060] Put 250g of purified water and 57g of AH01 into a 500mL flask, start stirring, and heat up to 80°C for 2.0 hours of hydrolysis reaction. After the reaction was completed, 65 g of 27% ammonia water (0.5007 mol) was added. Heat up to 80°C to dissolve, add 2g of activated carbon to decolorize for 0.5h, press filter while hot, and cool the filtrate to 25°C to grow crystals for 1h. The material was sucked and filtered to dryness, a...

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Abstract

The invention discloses a preparation method of xanthine. The preparation method comprises the following steps that 1, guanine performs diazo-reaction with sodium nitrite in a dilute acid or diazotized recovered mother solution; 2, after the diazo-reaction is completed, solid-liquid separation is performed, the step 3 is conducted on the obtained solid, and optionally the obtained liquid serves asthe diazotized recovered mother solution is reused in the step 1; 3, the solid obtained in the step 2 is subjected to hydrolysis reaction, and after reaction is completed, the xanthine is obtained posttreatment. The guanine is adopted as an initial raw material, the new preparation method is adopted, prepared diazonium salt is extracted from a system, the side reaction is inhibited, meanwhile reuse of the diazo-reaction mother solution is achieved, and the yield of three wastes is greatly reduced; in addition, a new refining method is adopted, so that the molar yield and product purity are far higher than literature values.

Description

technical field [0001] The invention belongs to the technical field of preparation of purine drug intermediates, and in particular relates to a preparation method of xanthine. Background technique [0002] Xanthines are mild stimulants and bronchodilators especially used to treat asthma symptoms. Derivatives of xanthines include caffeine, theophylline, theobromine, and mateine. [0003] The applicant is one of the main manufacturers of guanine in the world, with an annual output of more than 1,500 tons. Therefore, the technology of the present invention mainly relies on the guanine produced by the applicant as the starting material to prepare xanthine. [0004] Literature "Japanese Journal of Pharmaceutical Sciences" (Studies on Xanthine and Related Compounds.I: Syntheses of Xanthine from 4-Iminovioluric acid, Morizo ​​Ishidate, MinoruSekiya, Ichiro Kurita, Yakugaku Zasshi, 74 (4), p420, 1954) and patent literature DE834105 ( 1949) reported that xanthine was prepared by c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/04
CPCC07D473/04
Inventor 晏金华杨栽根张帅魏海鹏
Owner 潍坊奥通药业有限公司
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