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A kind of synthetic method of 9-ethyladenine

A technology for the synthesis of ethyl adenine and its synthesis method, which is applied in the field of synthesis of chemical organic substances, can solve the problems of complex synthesis procedures, environmental pollution, and low purity of synthetic products, and achieve high product purity, simple reaction steps, and low cost. Effect

Active Publication Date: 2020-03-31
肇东星湖生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing synthetic procedure of 9-ethyladenine is complex, some also pollute the environment, and the purity of the synthetic product is low

Method used

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  • A kind of synthetic method of 9-ethyladenine
  • A kind of synthetic method of 9-ethyladenine
  • A kind of synthetic method of 9-ethyladenine

Examples

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Embodiment 1

[0012] Embodiment 1: A kind of synthetic method of 9-ethyladenine

[0013] Take 27.03g of adenine, 24.11g of bromoethane, 27.63g of potassium carbonate, and 292.15g of N,N-dimethylformamide, heat to 40°C, and react for 8 hours; cool to room temperature, filter, remove potassium carbonate, and use 20.00 Wash the potassium carbonate filter cake with g N,N-dimethylformamide; collect the cleaning liquid into the filtrate, heat the filtrate to filter and dry it, and control the temperature at 90°C; add 348.17g of acetone, and heat to 55°C to dissolve the solid; stir Cool down to 10°C, and filter with suction to obtain a crude filter cake. Add 348.14 g of acetone to the solid, heat to 55°C to dissolve the solid; stir to cool down to 10°C, and filter with suction to obtain a refined filter cake. The refined filter cake was dried at 105°C to obtain 21.53g of 9-ethyladenine with a product purity of 99.6%. The liquid phase analysis diagram of the product is shown in figure 1 as shown,...

Embodiment 2

[0015] Take 27.08g of adenine, 24.21g of bromoethane, 27.62g of potassium carbonate, and 292.21g of N,N-dimethylformamide, heat to 40°C, and react for 8 hours; cool to room temperature, filter, remove potassium carbonate, and use 20.45 g N,N-dimethylformamide to clean the potassium carbonate filter cake; collect the cleaning liquid into the filtrate, heat the filtrate to filter and dry it, control the temperature at 90°C; add 348.31g of acetone, heat to 55°C to dissolve the solid; stir Cool down to 10°C, and filter with suction to obtain a crude filter cake. Add 348.28 g of acetone to the solid, heat to 55°C to dissolve the solid; stir to cool down to 10°C, and filter with suction to obtain a refined filter cake. The solid was dried at 105°C to obtain 22.35 g of 9-ethyladenine with a product purity of 99.7%. figure 2 The purity of the product of this example is proved. (VWD1A wavelength = 256nm)

Embodiment 3

[0017] Take 27.10g of adenine, 24.32g of bromoethane, 27.70g of potassium carbonate, and 292.31g of N,N-dimethylformamide, heat to 40°C, and react for 8 hours; cool to room temperature, filter, remove potassium carbonate, and use 20.24 g N,N-dimethylformamide to wash the potassium carbonate filter cake; collect the cleaning liquid into the filtrate, heat the filtrate to filter and dry it, and control the temperature at 90°C; add 348.14g of acetone, heat to 55°C to dissolve the solid; stir Cool down to 10°C, and filter with suction to obtain a crude filter cake. Add 348.27g of acetone to the solid, heat to 55°C to dissolve the solid; stir to cool down to 10°C, and filter with suction to obtain a refined filter cake. The solid was dried at 105°C to obtain 21.18g of 9-ethyladenine with a product purity of 99.5%. image 3 The purity of the product of this example is proved. (VWD1A wavelength = 256nm).

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Abstract

The invention relates to the technical field of the synthesis of chemical organic substance, in particular to a synthesis method of 9-ethyl adenine. The method comprises the following steps: feeding adenine, potassium carbonate and bromoethane into N, N-dimethyl formamide, performing heating reaction, performing centrifugation to remove the centrifugation, and concentrating and drying the filtrate; B, adding acetone into a product of the step A, heating, dissolving, purifying, cooling down, crystallizing and filtering, so as to obtain a 9-ethyl adenine crude filter cake; C, adding acetone to the 9-ethyl adenine crude filter cake of the step B, heating, dissolving, purifying, cooling down, crystallizing and filtering, so as to obtain a 9-ethyl adenine fine filter cake, and drying the fine filter cake, so as to obtain the 9-ethyl adenine. The method ensures that the purification of 9-ethyl adenine produced in the first step reaches greater than 85 percent, and the purify of 9-ethyl adenine reaches greater than 95 percent through the last two steps of refining. The method is simple in reaction steps, mild in operation conditions, and easy to control, does not cause any by-products during reaction, and is good in environmental protection property.

Description

technical field [0001] The invention relates to the technical field of synthesis of chemical organic substances, in particular to a synthesis method of 9-ethyladenine. Background technique [0002] 9-Ethyladenine, a derivative of adenine, is widely distributed in animal and plant tissues. 9-Ethyladenine is an intermediate in the synthesis of adefovir dipivoxil, and adefovir dipivoxil has strong inhibitory activity against hepatitis B virus. Studying the synthesis process of 9-ethyladenine is of great significance to the synthesis research of adefovir dipivoxil. The existing 9-ethyladenine synthesis procedures are complicated, some of which also pollute the environment, and the purity of the synthesized products is low. Contents of the invention [0003] In view of the above problems, the present invention provides a synthetic method of 9-ethyladenine which is environmentally friendly, low in cost and high in purity. [0004] In order to solve the above technical problem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D473/34
CPCC07D473/34
Inventor 曹侃朱文佳杨艳庆
Owner 肇东星湖生物科技有限公司