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Low-cost and high-yield adenine preparation method

A technology of adenine and epichlorohydrin, which is applied in the field of pharmaceutical biochemical industry, can solve the problems of large amount of three wastes, difficulty in industrial production, and high raw material prices, and achieve the effects of reducing production costs, increasing yields, and low product costs

Active Publication Date: 2016-02-24
XINFA PHARMA
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Problems solved by technology

The method has long reaction steps, cumbersome operation, and uses phosphorous oxychloride chlorination and iron powder reduction, resulting in a large amount of waste liquid after post-treatment, a large amount of three wastes to be treated, and is difficult for industrial production
[0006] Adenosine method: Lv Zhidong et al., Frontiers of Medicine 2012 No. 11 reported "Research on the new synthesis process of adenine from adenosine", using adenosine to prepare acetyl adenine through N-acetylation under acid catalysis, and then oxidized with hydrogen Preparation of adenine by hydrolysis of sodium aqueous solution, the raw material price of this method is high, it is not easy to obtain, and other acetylated by-products are easily produced during the acetylation of adenosine

Method used

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  • Low-cost and high-yield adenine preparation method

Examples

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Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1: the preparation of adenine

[0037] Add 50 grams of methanol, 9.3 grams (0.1 moles) of epichlorohydrin, 22.5 grams (0.33 moles) of 25% ammonia water in a 250 milliliter reactor with a tail gas absorption device, and react for 3 hours at 25 to 30 ° C; add 11.0 grams (0.11 moles) 30% formaldehyde, reacted at 25 to 30°C for 2 hours; added 15.0 grams (0.13 moles) of 30% hydrogen peroxide, and reacted at 25 to 30°C for 2 hours; slowly introduced 33.0 grams (0.46 moles ) chlorine gas, pass through, react at 25 to 30°C for 1 hour, add 35 grams (0.62 moles) of 30% ammonia water, and react at 25 to 30°C for 3 hours; add 6.8 grams (0.15 moles) of formamide, heat, and react at 85 to 90°C 2 hours, while recovering the distilled methanol; after recovering methanol, add 0.5 g of activated carbon, react at 80-85 ° C for 2- hours, filter while it is hot, cool the filtrate to 0-5 ° C, filter, and dry to obtain 10.5 g of light yellow solid gland Purine, yield 87.5%, HPLC p...

Embodiment 2

[0038] Embodiment 2: the preparation of adenine

[0039] The 50 g of methanol in Example 1 was replaced with 50 g of ethanol, and the rest were the same as in Example 1 to obtain 10.6 g of light yellow solid adenine with a yield of 88.3% and a HPLC purity of 99.1%.

Embodiment 3

[0040] Embodiment 3: the preparation of adenine

[0041] 50 grams of isopropanol was used instead of 50 grams of methanol in Example 1, and the rest were the same as in Example 1 to obtain 10.3 grams of light yellow solid adenine with a yield of 85.8% and a HPLC purity of 99.5%.

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Abstract

The invention relates to a low-cost and high-yield adenine preparation method. According to the method, epoxy chloropropane is adopted as a starting material, and ammonia water, formaldehyde, hydrogen peroxide, chlorine gas, ammonia water, and formamide are sequentially added for reaction to prepare adenine. In the method, raw materials are low in price and easy to obtain, the operation is simple, the use of phosphorus oxychloride is eliminated, the process is green, environment-friendly and low in cost, the product purity and the yield are high, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a low-cost and high-yield method for preparing adenine, which belongs to the technical field of pharmaceutical biochemical industry. Background technique [0002] Adenine (I), chemically named 6-aminopurine, is a component of nucleic acid and participates in the synthesis of genetic material. Adenine has important physiological functions, can promote the proliferation of leukocytes, and is used to prevent and treat leukopenia caused by various reasons, especially for leukopenia caused by tumor chemotherapy or other reasons. At the same time, adenine is also used to prepare medicines such as purine derivatives, and hundreds of tons of adenine are exported to the international market every year. [0003] There are three main methods for preparing adenine: the hypoxanthine method, the diethyl malonate method and the adenosine method. [0004] Hypoxanthine method: Document J.Med.Chem.1966, 9(1) 143-144 reported that hypoxanthine ...

Claims

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Application Information

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IPC IPC(8): C07D473/34
CPCC07D473/34
Inventor 戚聿新李新发吕强三王成威鞠立柱
Owner XINFA PHARMA
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