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Refining process of ethyl dihydrazone

A refining method, the technology of ethylenedihydrazone, applied in hydrazone preparation, organic chemistry, etc., can solve the problems of easy volatile loss of ethyl acetate, high production cost, and difficult extraction of the product, and achieve simple production process and low production cost Effect

Inactive Publication Date: 2010-06-23
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation process of this method needs to be extracted with ethyl acetate, and separated and purified by silica gel column chromatography, which is not suitable for industrial production
When extracting with ethyl acetate, due to the high solubility of ethylenedihydrazone in water, the product is not easy to be extracted completely, and ethyl acetate is also very easy to volatilize and lose, making the production cost higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] (1) At 60°C, the crude product of ethylenedihydrazone is dissolved in isopropanol, and the weight ratio of the crude product of ethylenedihydrazone to isopropanol is 1:3;

[0014] (2) The solution is crystallized at a low temperature of -50 to -40°C to obtain the product.

[0015] The crystallized product is separated by filtration and dried by vacuum drying.

Embodiment 2

[0017] The difference from Example 1 is that the crude product of ethylenedihydrazone is dissolved in n-propanol at 80° C., and the weight ratio of the crude product of ethylenedihydrazone to n-propanol is 1:5.

Embodiment 3

[0019] (1) At 80°C, the crude product of ethylenedihydrazone is dissolved in n-propanol, and the weight ratio of the crude product of ethylenedihydrazone to n-propanol is 1:4;

[0020] (2) The solution is crystallized at a low temperature of -10 to -5°C to obtain the product.

[0021] The crystallized product is separated by filtration and dried by vacuum drying.

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PUM

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Abstract

The present invention provides refining process of ethyl dihydrazone, and belongs to the field of chemical aldehydo hydrazone synthesizing technology. The refining process includes the following steps: dissolving coarse ethyl dihydrazone product in saturated C3 or C4 alcohol solution at 60-105 deg.c, and crystallizing at low temperature, with the C3 or C4 alcohol being n-propanol, isopropanol, n-butanol, isobutanol or their mixture. The present invention features the simplified production process and low production cost, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of aldehyde hydrazone chemical synthesis, in particular to a refining technology of ethylenedihydrazone. Background technique [0002] Ethylenedihydrazone is an important chemical raw material, which can be used to prepare 1-amino-1,2,3-triazole, and then 1,2,3-triazole and its derivatives. The method disclosed in US Patent No. 5,728,841 is as follows: 1.45 g of 40% aqueous solution of glyoxal, 1.00 g of hydrazine monohydrate and 10 mL of water are placed in a reaction vessel, and the mixture is stirred at room temperature for 1 h. It was then stirred at 100 °C for 3 h. After completion of the reaction, the solvent was distilled off under reduced pressure, the residue was extracted with ethyl acetate, and the extract was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was subjected to silica gel column chromatography to obtain 813 mg (94%) of ethyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C251/76C07C249/16
Inventor 吴玉凯周智明祝文秀于晓燕陈志恒孟子晖温鸿亮章军
Owner BEIJING INSTITUTE OF TECHNOLOGYGY