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A kind of preparation method of carbazate

A carbazate and methanol technology, which is applied in the field of carbazate preparation, can solve the problems of easy decomposition to generate nitrogen and water, difficult control of the synthesis process, complicated post-treatment process, etc., and achieve low operation difficulty and good Application value and application prospect, the effect of low raw material cost

Active Publication Date: 2021-02-26
HUNAN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Using carbonate and hydrazine hydrate as raw materials, the synthesis method of preparing carbazate by reaction is the main synthesis method at present, and the process has been continuously improved in recent years, but there are still many shortcomings in this synthesis method, such as harsh process requirements and cumbersome operation , complex post-treatment process, expensive raw materials, etc.
There is also a method of using sodium hypochlorite, urea and alcohol as raw materials to prepare methyl carbazate under the action of catalyst zinc or cadmium compound. The advantage of this method is that the raw material is cheap, but the sodium chloride of transition state urea formed by urea under the action of sodium hypochlorite Salt is very easy to decompose. When the mixing speed of the reaction materials or the reaction temperature and reaction time fluctuate, the sodium chloride salt of the transition state urea is easy to decompose to generate nitrogen and water, which makes the synthesis process difficult to control, and there are certain difficulties in industrial design and operation. There are still problems such as difficult operation and difficult control

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  • A kind of preparation method of carbazate

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Embodiment 1

[0027] A preparation method of carbazate, comprising the following steps:

[0028] Potassium hydroxide is used to adjust the pH of the aqueous solution of 120.1g urea (the mass fraction of urea in the aqueous solution of urea is 50%, that is, the solution contains 1mol urea). The aqueous solution of 421g calcium hypochlorite (the mass fraction of calcium hypochlorite in this aqueous solution of calcium hypochlorite is 17%, promptly contains 0.5mol calcium hypochlorite in the solution), adds 0.6g magnesium chloride powder and 64.1g (2mol) methyl alcohol , after stirring evenly, the temperature of the obtained mixed solution was raised to 50°C, and reacted for 1 hour. After the reaction was completed, the excess methanol in the system was removed under reduced pressure, extracted twice with dichloroethane at a temperature of 50°C, and the extracts were combined. The temperature was lowered to 0° C. to crystallize, and filtered to obtain 89.1 g of white crystalline particles, the...

Embodiment 2

[0030] A preparation method of carbazate, comprising the following steps:

[0031] Potassium hydroxide is used to adjust the pH of the aqueous solution of 120.1g urea (the mass fraction of urea in the aqueous solution of urea is 50%, that is, the solution contains 1mol urea). The aqueous solution of 421g calcium hypochlorite (massfraction 17% of calcium hypochlorite in this aqueous solution of calcium hypochlorite, promptly contains 0.5mol calcium hypochlorite in the solution), adds 12g magnesium chloride powder and 64.1g (2mol) methyl alcohol, After stirring evenly, raise the temperature of the obtained mixture to 50°C, react for 1 hour, remove excess methanol in the system under reduced pressure after the reaction, extract twice with dichloroethane at a temperature of 50°C, combine the extracts, and cool down Crystallize at 0°C and filter to obtain 88.0 g of white crystalline particles, the content of methyl carbazate in the white crystalline particles is 98.3%, and the yiel...

Embodiment 3

[0033] A preparation method of carbazate, comprising the following steps:

[0034] Potassium hydroxide is used to adjust the pH of the aqueous solution of 120.1g urea (the mass fraction of urea in the aqueous solution of urea is 50%, that is, the solution contains 1mol urea). The aqueous solution of 421g calcium hypochlorite (the mass fraction of calcium hypochlorite in this aqueous solution of calcium hypochlorite is 17%, promptly contains 0.5mol calcium hypochlorite in the solution), adds 0.6g magnesium chloride powder and 92.1g (2mol) ethanol After stirring evenly, the resulting mixture was heated to 50°C and reacted for 2 hours. After the reaction, the excess ethanol in the system was removed under reduced pressure, extracted twice with dichloroethane at a temperature of 50°C, and the extracts were combined. The temperature was lowered to 0° C. to crystallize, and filtered to obtain 99.2 g of off-white crystalline particles, the content of ethyl carbazate in the white crys...

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Abstract

The invention discloses a method for preparing carbazate. The preparation method uses calcium hypochlorite, urea and alcohol as raw materials to prepare carbazate under the catalysis of magnesium chloride. In the preparation method of the present invention, urea reacts under the action of calcium hypochlorite to generate calcium chloride salt of transition state urea which has stable properties and is not easy to decompose, so that the synthesis process is easier to control, and the reaction can be carried out under safer conditions. Then, under the catalysis of magnesium chloride, the calcium chloride salt of transition state urea is reacted with alcohol to prepare carbazate with high content and high yield. The preparation method of the present invention has the advantages of simple process, convenient operation, low cost of raw materials, mild reaction conditions, safety, high product content, high yield, etc. The method is beneficial to industrial production and has good application value and application prospect.

Description

technical field [0001] The invention relates to a preparation method of carbazate. [0002] technical background [0003] Carbazate is an important class of chemical raw materials. For example, methyl carbazate can be used to synthesize antitumor drug naphthalimide derivatives, pesticide carbadox, etc.; ethyl carbazate can be used to synthesize cardiovascular and cerebrovascular drugs. Turoperazine, cross-linking curing agent tris (2-methylaziridine) phosphine oxide, etc.; isopropyl carbazate is used to synthesize organic compounds of oxadiazoles. [0004] Using carbonate and hydrazine hydrate as raw materials, the synthesis method of preparing carbazate by reaction is the main synthesis method at present, and the process has been continuously improved in recent years, but there are still many shortcomings in this synthesis method, such as harsh process requirements and cumbersome operation , The post-processing process is complicated, and the raw materials are expensive. T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C281/02
CPCC07C281/02
Inventor 周勇李萍周锦萍王燕黄炜黄幼援臧阳陵
Owner HUNAN CHEM RES INST