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A kind of preparation method of oxymethylisourea acetate

A technology of oxymethyl isourea hydrogen sulfate and oxymethyl isourea, applied in the field of preparation of oxymethyl isourea acetate, can solve the problems of poor yield, difficult to remove, difficult to separate and remove, etc. The effect of high purity, high yield and simple process

Inactive Publication Date: 2011-12-21
JUHUA GRP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that oxymethylisourea is hydrolyzed into methanol and urea, the latter is difficult to separate and remove, and decomposes when the aqueous solution of oxymethylisourea is concentrated, so only urea containing many impurities can be obtained in extremely poor yield. Oxymethylisourea acetate
The disadvantage of this method is that the by-product sodium chloride has a certain solubility in methanol and is difficult to completely remove
The shortcoming of this method is: the reaction of oxymethylisourea hydrogen salt and sodium hydroxide is incomplete, and the ratio of acetic acid dripping is difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Put 292.4Kg (1.7Kmol) oxymethylisourea bisulfate (95.5%), 150Kg (1.83Kmol) sodium acetate and 68Kg (1.7Kmol) sodium hydroxide in 446Kg (14Kmol) methanol, and at 30°C After stirring for 5 hours, filter, rinse the filter residue with a small amount of methanol, and put the filtrate into the concentration kettle, and concentrate it in vacuum at 60°C. The concentrated solution enters the crystallization kettle to crystallize. Finally, 165 Kg (75.9%) of oxymethylisourea acetate with a purity of 98% was obtained.

Embodiment 2

[0019] Put 292.4Kg (1.7Kmol) oxymethylisourea bisulfate (95.5%), 145Kg (1.77Kmol) sodium acetate and 70Kg (1.75Kmol) sodium hydroxide in 446Kg (17Kmol) methanol, and at 40°C Stir for 8 hours and then filter, rinse the filter residue with a small amount of methanol, put the filtrate into the concentration kettle, and concentrate in vacuum at 70°C, the concentrated solution enters the crystallization kettle for crystallization, filter after crystallization, and dry the product in vacuum at 50°C Finally, 160 Kg (73.6%) of oxymethylisourea acetate with a purity of 98% was obtained.

Embodiment 3

[0021] Put 292.4Kg (1.7Kmol) oxymethylisourea bisulfate (95.5%), 140Kg (1.7Kmol) sodium acetate and 70Kg (1.75Kmol) sodium hydroxide in 446Kg (14Kmol) methanol, and at 20°C After stirring for 4 hours, filter, rinse the filter residue with a small amount of methanol, and put the filtrate into the concentration tank, and concentrate it in vacuum at 65°C. The concentrated solution enters the crystallization tank for crystallization. Finally, 155 Kg (71.3%) of oxymethylisourea acetate with a purity of 98% was obtained.

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Abstract

The invention discloses a preparation method of oxymethylisourea acetate. The method comprises the following steps: 1) the methanol solution of oxymethylisourea hydrogen sulfate is reacted with sodium acetate and sodium hydroxide at a temperature of 10°C to 65°C, and the reaction time is 2 hours to 10 hours, and oxymethylisourea hydrogen sulfate The molar ratio of salt to sodium hydroxide and methanol is 1:1:6~10, and the molar ratio of oxymethylisourea bisulfate to sodium acetate and sodium hydroxide is 1:0.8~1.5:0.8~1.50; 2) The precipitated sodium sulfate is removed from the reaction mixture at the temperature of step 1); 3) the reaction solution is concentrated by distilling methanol at a temperature of 40°C to 80°C; 4) the oxymethylisourea acetate concentrate is cooled, Crystallization, centrifugation can be. The synthesized product of the invention has high purity, high yield and simple process, and the method is particularly suitable for industrial scale application.

Description

technical field [0001] The invention relates to a preparation method of oxymethylisourea acetate. Background technique [0002] Oxymethylisourea salt of strong mineral acid can be obtained by reacting urea with dimethyl sulfate, acidolysis and hydrolysis. A typical example is oxymethylisourea hydrogen sulfate. [0003] However, oxymethylisourea bisulfate cannot react with acetic acid, because the strength of acetic acid is too weak to directly obtain weakly acidic oxymethylisourea salt. [0004] The active ingredient of oxymethylisourea acetate, oxymethylisourea, is an important intermediate for the synthesis of fluorouracil antitumor drugs. It can also be used as an amidinating agent to react with amines to generate corresponding guanidine salts. Many active ingredients of drugs or plant protection agents with a guanidine structure contain acetate as an anion, and oxymethylisourea acetate is needed as an guanylation agent, such as oxymethylisourea acetate reacts with dod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C275/70C07C273/18
Inventor 周晓红姜永清
Owner JUHUA GRP
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