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Heating synthesis method of uracil

A synthetic method and technology of uracil, which is applied in the field of uracil synthesis, can solve the problems of high equipment requirements, difficult separation of intermediates, and difficult availability of raw materials, and achieve the effects of good selectivity, low pollution, and easy liquid separation

Active Publication Date: 2021-10-01
河北广兴化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, although there are many literature reports on the chemical synthesis of uracil, these synthetic methods are either difficult to separate the intermediates and have low yields; or the raw materials are not easy to obtain, and the synthetic route is long; or there are environmental pollution problems and high requirements for equipment.

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  • Heating synthesis method of uracil

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Effect test

Embodiment 1

[0024] In embodiment 1, the thermal synthesis method of uracil comprises the following steps:

[0025] S1. Add an organic solvent, acetic anhydride and urea into the reaction vessel, and mix and react, wherein the reaction temperature is 25° C., and the reaction time is 2 hours;

[0026] S2, then add acetaldehyde and alkali to the reaction container, and add a catalyst to carry out condensation cyclization reaction, wherein the reaction temperature is 45 ° C, the reaction time is 2h, to obtain uracil;

[0027] In S1, the mol ratio of acetic anhydride and urea is 2.1:1, and described organic solvent is an inert organic solvent;

[0028] In S2, the mol ratio of acetaldehyde and urea is 1.3:1, and wherein alkali is ammoniacal liquor, and the mol ratio of ammonia in ammoniacal liquor and urea is 1.6:1, and described catalyzer is light microsphere catalyst, and catalyst add-on is urea quality 3%.

[0029] Further, the preparation method of the lightweight microsphere catalyst inc...

Embodiment 2

[0037] In embodiment 2, the thermal synthesis method of uracil comprises the following steps:

[0038] S1. Add an organic solvent, acetic anhydride and urea into the reaction vessel, and perform a mixed reaction, wherein the reaction temperature is 35° C., and the reaction time is 4 hours;

[0039] S2, then add acetaldehyde and alkali to the reaction vessel, and add a catalyst to carry out condensation cyclization reaction, wherein the reaction temperature is 65 ° C, the reaction time is h, to obtain uracil;

[0040] In S1, the mol ratio of acetic anhydride and urea is 2.4:1, and described organic solvent is an inert organic solvent;

[0041] In S2, the mol ratio of acetaldehyde and urea is 1.5:1, and wherein alkali is ammoniacal liquor, and the mol ratio of ammonia in ammoniacal liquor and urea is 1.9:1, and described catalyzer is light microsphere catalyst, and catalyst add-on is urea quality 5%.

[0042] Further, the preparation method of the lightweight microsphere catal...

Embodiment 3

[0050] In embodiment 3, the thermal synthesis method of uracil comprises the following steps:

[0051] S1. Add an organic solvent, acetic anhydride and urea into the reaction vessel, and perform a mixed reaction, wherein the reaction temperature is 30° C., and the reaction time is 3 hours;

[0052] S2, then add acetaldehyde and alkali to the reaction container, and add a catalyst to carry out condensation cyclization reaction, wherein the reaction temperature is 55 ° C, the reaction time is 4h, to obtain uracil;

[0053] In S1, the mol ratio of acetic anhydride and urea is 2.3:1, and described organic solvent is an inert organic solvent;

[0054] In S2, the mol ratio of acetaldehyde and urea is 1.4:1, and wherein alkali is ammoniacal liquor, and the mol ratio of ammonia in ammoniacal liquor and urea is 1.8:1, and described catalyzer is light microsphere catalyst, and catalyst add-on is urea quality 4%.

[0055] Further, the preparation method of the lightweight microsphere cat...

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Abstract

The invention relates to the technical field of uracil synthesis, in particular to a heating synthesis method of uracil, which comprises the following steps: S1, adding an organic solvent, acetic anhydride and urea into a reaction container, mixing and reacting at the reaction temperature of 25-35 DEG C for 2-4 hours; S2, adding acetaldehyde and alkali into the reaction container, adding a catalyst, performing condensation cyclization reaction, the reaction temperature being 45-65 DEG C, the reaction time being 2-6 h, to obtain the uracil. The heating synthesis method of the uracil has the advantages that raw materials are cheap and easy to obtain, synthesis steps are simple, the yield of the uracil is high, pollution is small, and the heating synthesis method is suitable for application and popularization.

Description

technical field [0001] The invention relates to the technical field of uracil synthesis, in particular to a heating synthesis method of uracil. Background technique [0002] Uracil is an important intermediate in fine chemicals, pesticides and medicine, especially in the field of medicine, mainly used in the synthesis of anti-AIDS drugs and anti-hepatitis B drugs such as uridine, fluorouracil, iodine glycosides, and fluterol, which are widely used. In the past two decades, pyrimidine nucleoside antiviral drugs have developed rapidly. There are tens of thousands of compounds with certain antiviral activity using uracil as an intermediate, and 26 drugs are currently used in clinical practice. With the development of the pharmaceutical industry, the demand for uracil will increase. [0003] At present, although there are many literature reports on the chemical synthesis of uracil, these synthetic methods are either difficult to separate the intermediates and have low yields; o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/54B01J23/72B01J35/08
CPCC07D239/54B01J23/72B01J35/51Y02P20/584
Inventor 韩伟
Owner 河北广兴化工有限公司
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