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Microwave-assisted high-efficiency method for synthesizing 5-cyanouracil

A cyanuridine and microwave-assisted technology, which is applied in the field of microwave-assisted efficient synthesis of cyanide-containing uracil, can solve the problems of long reaction time, complicated operation, high raw material cost, etc., and achieve the effect of low cost, simple operation and high yield

Active Publication Date: 2015-02-18
ZUNYI MEDICAL UNIVERSITY
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Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of efficient, green 5-cyanuridine synthetic method for existing deficiency of 5-cyanuracil synthetic method, the inventive method has overcome the weak point of prior art, as already reported The method for synthesizing 5-cyanuracil has many problems such as lengthy reaction time, complicated operation and high cost of raw materials. By simplifying and optimizing the reaction conditions, a 5-cyanuridine with high efficiency, mild reaction conditions, simple operation and high yield is provided. Synthetic method of uracil

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  • Microwave-assisted high-efficiency method for synthesizing 5-cyanouracil

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[0019] A method for microwave-assisted high-efficiency synthesis of 5-cyanuracil, consisting of the following steps:

[0020] Step 1: microwave 1-300mmol of urea, 1-300mmol of malononitrile and 10-80 mL of triethyl orthoformate at a microwave reaction temperature of 60°C-80°C, a microwave power of 500W, and normal pressure, and microwave for 8-20 minutes. Prepare dicyanide intermediate I;

[0021] The reaction equation is:

[0022] ;

[0023] Step 2: Filter the reaction system of step 1 to remove the remaining triethyl orthoformate, then dissolve the obtained solid in 5-50 mL of sodium ethoxide 1.0-2.0 mol / L solution, and microwave at a reaction temperature of 30-50°C and power 300W, under the condition of normal pressure, carry out radiation reaction for 30-50 minutes; add 0.1-0.5 g of activated carbon for decolorization, then acidify with 5-30mL of glacial acetic acid and filter the resulting precipitate to obtain intermediate II;

[0024] Step 3: Add 30-150mL of 2.5-3....

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Abstract

The invention relates to a microwave-assisted high-efficiency method for synthesizing 5-cyanouracil, which comprises the following steps: carrying out microwave radiation on urea, malononitrile and triethyl orthoformate at the microwave reaction temperature of 60-80 DEG C under the microwave power of 500W under atmospheric pressure for 8-20 minutes, and filtering the residual triethyl orthoformate out of the reaction system to obtain a dicyan intermediate I; dissolving the obtained solid in a sodium ethylate 1.0-2.0 mol / L solution, carrying out radiation reaction at the microwave reaction temperature of 30-50 DEG C under the microwave power of 300W under atmospheric pressure for 30-50 minutes, adding activated carbon for decolorization, filtering, and acidifying the filtered precipitate with glacial acetic acid to obtain an intermediate II; and adding 2.5-3.0 mol / L dilute hydrochloric acid into the intermediate II, carrying out radiation at the microwave reaction temperature of 80-100 DEG C under the microwave power of 500W under atmospheric pressure for 30-50 minutes, cooling, and filtering to obtain the 5-cyanouracil.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical chemical synthesis, in particular to a method for preparing cyanide-containing uracil compounds, in particular to a microwave-assisted method for efficiently synthesizing cyanide-containing uracil. Background technique [0002] 5-Cyanouracil is a chemically synthesized 5-fluorouracil analogue that inhibits pyrimidine catabolism. In addition, the pyrimidinone in its structure has a similar structure to many phosphodiesterase inhibitors, which is expected to have potential efficacy in cardiotonic drugs. At present, its market price is 1200-1500 yuan / g, and the high market price limits its further chemical modification to discover new lead compounds and pharmacological activity research. [0003] Existing bibliography reports the synthetic method of 5-cyanuracil at present, but these methods are many at high temperature 130 degrees, reaction time is long, operation is numerous and diverse, us...

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Application Information

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IPC IPC(8): C07D239/557
CPCC07D239/47C07D239/557
Inventor 袁泽利何顺莉宋文婷余光勤
Owner ZUNYI MEDICAL UNIVERSITY
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