Uracil heating synthesis method

A synthesis method and technology of uracil, applied in the field of uracil synthesis, can solve the problems of restricting product production scale, low product yield and high sulfuric acid concentration, and achieve the effects of shortening reaction time, shortening condensation time and reducing environmental pollution

Active Publication Date: 2018-03-13
HENAN VOCATIONAL COLLEGE OF APPLIED TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has the defects of long heating time, low product yield, high sulfuric acid concentration and large dosage in production, which seriously restricts the production scale of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The present embodiment provides a kind of thermal synthesis method of uracil, and its steps comprise:

[0024] Condensation Add 1800 kg of oleum containing 10% sulfur trioxide in an acid-resistant reaction kettle with a capacity of 5 tons, and add 1 g of oleum to the oleum under stirring. Add 120 kg of urea to the oleum, then add 250 kg of malic acid to the fuming sulfuric acid under stirring conditions at a rate of 10 g per second, and use microwave equipment to heat it to condense at 90°C React for 30 minutes;

[0025] Crystallization Add 2500 L of water to the acid-resistant reaction kettle under stirring conditions, release the reaction solution after cooling down to room temperature, and filter to obtain crude uracil;

[0026] Refining Add the uracil crude product into another reaction kettle with a capacity of 5 tons, and add 3000 L of water and 30 kg of activated carbon to it to obtain an adsorption mixed solution, heat the adsorbed mixed solution to boiling and...

Embodiment 2

[0030] The present embodiment provides a kind of heating synthetic method of uracil, and its step is roughly the same as the step in embodiment 1, and difference is:

[0031] The mass ratio of the oleum, the urea and the malic acid in the condensation step in this embodiment is 33:2:5; the temperature of microwave heating is 85°C, and the condensation time is 35 min; The addition of said urea in said fuming hydrochloric acid is 2 g per second, and the addition of said malic acid is 10 g per second.

[0032] It has been determined that the yield of finished uracil produced by the heating synthesis method provided in this example is 70.2%, and the amount of oleum used is 10% less than that used in the water-bath heating condensation reaction process.

Embodiment 3

[0034] The present embodiment provides a kind of heating synthetic method of uracil, and its step is roughly the same as the step in embodiment 1, and difference is:

[0035] The mass ratio of the oleum, the urea and the malic acid in the condensation step in this embodiment is 40:5:7; the microwave heating temperature is 85°C, and the condensation time is 33 min; the The mass percent of sulfur trioxide contained in the oleum is 8%; the per-second addition of the urea to the fuming hydrochloric acid is 2.5 g, and the per-second addition of the malic acid is 20 g.

[0036] It has been determined that the yield of finished uracil produced by the heating synthesis method provided in this example is 70.0%, and the amount of oleum used is 11.1% less than that used in the water-bath heating condensation reaction process.

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Abstract

The invention provides uracil heating synthesis method. The method comprises the following step that materials including oleum containing sulfur trioxide with the mass percent being 8 to 12 percent, urea and malic acid are proportioned according to the mass ratio of (30 to 40):(1 to 5):(3 to 7); under the stirring condition, the urea is firstly added into the oleum; then, the malic acid is added into the oleum to obtain a mixed material; the mixed material is subjected to microwave heating, so that the mixed material is subjected to condensation reaction at the temperature of 85 to 90 DEG C; acondensation material is obtained; the condensation material is mixed with water; filtering is performed to obtain a uracil crude product. The heating synthesis method provided by the invention has the advantages that the steps are simple; the consumed time is short; the yield of the produced uracil product is high; the production cost is low; the pollution is reduced.

Description

technical field [0001] The invention belongs to the technical field of uracil synthesis, in particular, the invention relates to a heating synthesis method of uracil. Background technique [0002] The chemical name of uracil is 2,4-(1H,3H)-pyrimidinedione or 2,4-dihydroxypyrimidine. Molecular formula is C 4 h 4 N 2 o 2 . Uracil can be used as a drug to treat digestive system cancer, breast cancer and thyroid cancer, etc., and it has a good effect on advanced gastric cancer in combination with mitomycin; and uracil can be used as a pharmaceutical intermediate to synthesize 5-fluorouracil, Tegafur, bisfurfururacil, doxifluridine, carmofur, 5-iodo-2'-deoxyuridine. [0003] At present, the industrialized production of uracil is mainly in the fuming sulfuric acid containing 15% sulfur trioxide by mass percentage, using malic acid and urea as raw materials, heating and stirring in a steam bath for 4 hours, then crystallization, activated carbon decolorization, and finally re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/54
CPCC07D239/54
Inventor 韩宝来龚子东王文静陈永惠李元元张香菊刘伟芬李东
Owner HENAN VOCATIONAL COLLEGE OF APPLIED TECH
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