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Synthetic method of 2-chloroethyl hydrazono methyl formate

A technology of chloroethyl hydrazide and methyl formate, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve complex processes, many by-products, and hydrogen chloride environment Harm and other problems, to achieve the effect of high catalytic activity, improved conversion and yield, and improved catalytic ability

Inactive Publication Date: 2019-01-11
XUZHOU NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Methyl 2-chloroethyl hydrazonocarboxylate (structural formula: ClCH 2 CH=NNHCOCH 3 ) is an important organic chemical intermediate. The traditional synthesis method is to generate methyl thioformate by chlorinating methyl thioformate and methanol under the action of pyridine, and then react with hydrazine to prepare methyl carbazate. However, the process uses Methyl chlorinated thioformate, which is harmful to the human body, is used as raw material, and the by-product hydrogen chloride has the disadvantages of serious environmental hazards, complicated process, and many by-products.

Method used

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Examples

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Effect test

Embodiment 1

[0017] A kind of synthetic method of methyl 2-chloroethyl hydrazonocarboxylate, it is characterized in that the method comprises the following steps:

[0018] Step 1. Add 18g of dimethyl carbonate, 30g of hydrazine hydrate and 2g of AZO-CMP-1 catalyst in a 50ml round bottom flask, heat to reflux for 5h, filter out the catalyst powder while hot and then distill at atmospheric pressure to steam out the product methanol and excess dimethyl carbonate;

[0019] Step 2. Add 36 g of chloroacetaldehyde with a concentration of 10% to the above system, stir, and after cooling in an ice-water bath, slowly add 45 g of an aqueous solution of methyl formate with a concentration of 50%. Maintain the internal temperature at 0°C, a large amount of white solid is formed;

[0020] Step 3. After the dropwise addition, stir for 10 minutes to remove the ice-water bath, continue to stir at room temperature for 30 minutes and filter with suction, wash the solid with 25ml of distilled water for 3 tim...

Embodiment 2

[0029] Step 1. Add 15g of dimethyl carbonate, 30g of hydrazine hydrate and 2g of AZO-CMP-1 catalyst in a 50ml round bottom flask, heat to reflux for 5h, filter out the catalyst powder while hot and then distill at atmospheric pressure to steam out the product methanol and excess The dimethyl carbonate; All the other steps are with embodiment 1.

Embodiment 3

[0031] Step 1. Add 12g of dimethyl carbonate, 30g of hydrazine hydrate and 2g of AZO-CMP-1 catalyst in a 50ml round bottom flask, heat to reflux for 5h, filter out the catalyst powder while hot and then distill at atmospheric pressure to steam out the product methanol and excess The dimethyl carbonate; All the other steps are with embodiment 1.

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Abstract

The invention discloses a synthetic method of 2-chloroethyl hydrazono methyl formate. According to the synthetic method, dimethyl carbonate, hydrazine hydrate, chloroacetaldehyde, methyl formate, p-nitrobenzaldehyde, acetic anhydride, pyrrole, pyridine, zinc chloride, and terephthalaldehyde are taken as main raw materials; dimethyl carbonate and hydrazine hydrate are subjected to oxidation reaction under the effect of catalyst AZO-CMP-1; chloroacetaldehyde and methyl formate addition substation is carried out so as to obtain the target product 2-chloroethyl hydrazono methyl formate; in oxidation reaction, the catalyst is a liquid solid double-phase catalyst system, and is extremely high in catalytic activity, selectivity, and recycling stability; high conversion degree is achieved; production separation purifying is easy; and product yield is high.

Description

technical field [0001] The invention relates to a method for synthesizing methyl 2-chloroethyl hydrazonocarboxylate, which belongs to the field of chemical synthesis. Background technique [0002] Methyl 2-chloroethyl hydrazonocarboxylate (structural formula: ClCH 2 CH=NNHCOCH 3 ) is an important organic chemical intermediate. The traditional synthesis method is to generate methyl thioformate by chlorinating methyl thioformate and methanol under the action of pyridine, and then react with hydrazine to prepare methyl carbazate. However, the process uses Methyl chlorinated thioformate, which is harmful to human body, is used as raw material, and the by-product hydrogen chloride has the disadvantages of serious environmental hazards, complicated process, and many by-products. It is urgent to design a new reaction route to effectively avoid the environmental hazards caused by the oxidation of methyl thioformate. By using a suitable catalyst, the process has a high degree of co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C281/04B01J31/22
CPCB01J31/181B01J31/2213C07C281/04
Inventor 陆玉萍孟建张文
Owner XUZHOU NORMAL UNIVERSITY
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