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Synthesis method of carbohydrazide

A synthetic method, carbohydrazide technology, applied in organic chemistry, etc., can solve problems such as high safety operation requirements, toxic raw materials, and toxic by-products, and achieve high yield, fast reaction speed, and less side reactions.

Pending Publication Date: 2022-02-11
DONGGUAN UPC IND & TRADE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For this reason, the present invention provides a synthetic method of carbohydrazide to solve the problems of toxic raw materials, high requirements for safe operation, and generation of toxic by-products in existing synthetic methods of carbohydrazide.

Method used

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  • Synthesis method of carbohydrazide
  • Synthesis method of carbohydrazide
  • Synthesis method of carbohydrazide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A kind of synthetic method of carbohydrazide comprises the steps:

[0031] Step 1: First add 56.28g of 80% hydrazine hydrate solution to a 500ml three-necked flask, then add 90.09g of 99.9% dimethyl carbonate, turn on the magnetic stirrer, and react for 2 hours at a reaction temperature of 70°C to synthesize Methyl carbazate crude product; the synthesized methyl carbazate crude product is cooled to room temperature, weighs 142.97g of the reaction solution, uses a single-necked flask to evaporate and crystallize under reduced pressure, and distills out 65.11g of the mother liquor to obtain 77.86g of the product. The product is tested by GC, and the test results are as follows: image 3 As shown, it can be seen that the product obtained is methyl carbazate, and the product purity is 98.3%, and the product yield obtained by calculation is 96.04%.

[0032] Step 2: First add 78.29g of 80% hydrazine hydrate solution to a 500ml three-necked flask, then add 45.04g of 98.3% met...

Embodiment 2

[0034] A kind of synthetic method of carbohydrazide comprises the steps:

[0035] Step 1: First add 56.35g of 80% hydrazine hydrate solution into a 500ml three-neck flask, then add 90.13g of 99.9% dimethyl carbonate, turn on the magnetic stirrer, and react for 2 hours at a reaction temperature of 60°C to synthesize hydrazine groups Crude methyl formate; cool the synthesized crude methyl carbazate to room temperature, weigh 142.64 g of the reaction solution, use a single-necked flask to evaporate and crystallize under reduced pressure, distill 63.09 g of the mother liquor, and obtain 79.55 g of the methyl carbazate product, The product purity is 98.8%, and the yield is 98.1%.

[0036] Step 2: First add 60.07g of 80% hydrazine hydrate solution to a 500ml three-neck flask, then add 72.07g of 98.8% methyl carbazate, turn on the magnetic stirrer, and react for 6 hours at a reaction temperature of 85°C to synthesize carbon Crude hydrazide: cool the synthesized crude carbohydrazide ...

Embodiment 3

[0038] A kind of synthetic method of carbohydrazide comprises the steps:

[0039] Step 1: First add 56.31g of 80% hydrazine hydrate solution to a 500ml three-necked flask, then add 90.08g of 99.9% dimethyl carbonate, turn on the magnetic stirrer, and react for 2 hours at a reaction temperature of 50°C to synthesize hydrazine groups Crude methyl formate; cool the synthesized crude methyl carbazate to room temperature, weigh 143.65 g of the reaction solution, use a single-necked flask to evaporate and crystallize under reduced pressure, and distill 64 g of the mother liquor to obtain 79.65 g of the methyl carbazate product. The purity is 99.1%, and the yield is 98.2%.

[0040] Step 2: First add 78.35g of 80% hydrazine hydrate solution to a 500ml three-neck flask, then add 45.08g of 99.1% methyl carbazate, turn on the magnetic stirrer, and react for 5 hours at a reaction temperature of 85°C to synthesize carbon Hydrazide crude product: cool the synthesized carbohydrazide crude p...

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Abstract

The invention discloses a synthesis method of carbohydrazide, and relates to the technical field of chemical synthesis, the synthesis method comprises the following steps: 1, synthesizing a methyl carbazate crude product by using dimethyl carbonate and hydrazine hydrate as raw materials; and performing reduced pressure distillation on the synthesized methyl carbazate crude product, and drying to obtain methyl carbazate; 2, synthesizing a carbohydrazide crude product by taking hydrazine hydrate and methyl carbazate obtained in the step 1 as raw materials; and carrying out reduced pressure distillation on the synthesized carbohydrazide crude product, and drying to obtain the carbohydrazide. According to the synthesis method of carbohydrazide, dimethyl carbonate and hydrazine hydrate serve as raw materials, carbohydrazide is synthesized at low temperature through a two-step method, the adopted raw materials are non-toxic and environmentally friendly, the whole reaction process is mild in condition, easy to control and high in reaction speed, and the obtained product is high in yield, few in side reaction and easy to purify.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis method of carbohydrazide. Background technique [0002] Carbohydrazide is an important intermediate in organic synthesis, which can be used to synthesize a series of biologically active heterocyclic compounds. Carbohydrazide is also a boiler feed water oxygen scavenger that has gradually been widely recognized and applied in recent years. Its oxygen scavenging mechanism is similar to that of hydrazine, but its ability to scavenge oxygen and passivate the surface of iron and copper metals is significantly better than that of hydrazine. Ammonia, and less toxic than hydrazine, easy to transport. In addition, carbohydrazide can also be used as a component of rocket propellant, color development, etc., and has a wide range of uses. [0003] The traditional carbohydrazide synthesis method is to use carbonyl chloride and hydrazine to react. This method is not on...

Claims

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Application Information

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IPC IPC(8): C07C281/02C07C281/06
CPCC07C281/02C07C281/06
Inventor 刘晨旭杨文兵郭云山刘伟成
Owner DONGGUAN UPC IND & TRADE
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