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Process for purifying tert-butylhydrazine hydrochloride

A technology of tert-butylhydrazine and hydrochloride, which is applied in the field of pesticide intermediates and pesticides, can solve the problems of increasing the difficulty of purification of downstream products, waste of raw materials, and insignificant changes in solubility with temperature, etc.

Inactive Publication Date: 2018-12-21
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The presence of hydrazine hydrochloride leads to waste of raw materials in the production of downstream products; introduces new impurities in downstream products; increases the difficulty of purification of downstream products
[0004] Due to the high solubility of tert-butylhydrazine hydrochloride in water, and the solubility does not change significantly with temperature, the conventional recrystallization method is used for purification, and the yield is low

Method used

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  • Process for purifying tert-butylhydrazine hydrochloride
  • Process for purifying tert-butylhydrazine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 100mL three-neck flask equipped with a stirring device, add 10.00g of 89.36% (w / w) tert-butylhydrazine hydrochloride and 20mL of absolute ethanol respectively, stir for 30 minutes, cool to 4°C, and add 2.00g of ferric chloride g. React at 4°C for 2 hours, filter immediately after the reaction, wash the filter cake with a small amount of cold ethanol, and dry to obtain 7.15 g of white powder with a yield of 80.01%. As determined by high performance liquid chromatography, the content of tert-butylhydrazine hydrochloride is 98.06%.

Embodiment 2

[0020] In a 100mL three-necked flask equipped with a stirring device, add 8.00g of 89.36% (w / w) tert-butylhydrazine hydrochloride and 20mL of 90% (v / v) ethanol respectively, stir for 20 minutes, cool to 0°C, add Ferric chloride 0.80g. React at 0°C for 2 hours, filter immediately after the reaction, wash the filter cake with a small amount of cold ethanol, and dry to obtain 5.91 g of white powder with a yield of 82.67%. As determined by high performance liquid chromatography, the content of tert-butylhydrazine hydrochloride is 98.67%.

Embodiment 3

[0022] In a 100mL three-necked flask equipped with a stirring device, add 6.00g of 89.36% (w / w) tert-butylhydrazine hydrochloride and 20mL of 80% (v / v) ethanol respectively, stir for 10 minutes, cool to 2°C, add Ferric chloride 1.50g. React at 2°C for 3 hours, filter immediately after the reaction, wash the filter cake with a small amount of cold ethanol, and dry to obtain 4.18 g of white powder with a yield of 77.96%. As determined by high performance liquid chromatography, the content of tert-butylhydrazine hydrochloride is 98.52%.

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Abstract

The invention belongs to the field of pesticides and pesticide intermediates and discloses a process for purifying tert-butylhydrazine hydrochloride. The process disclosed by the invention comprises the following operating steps: respectively adding ethanol and tert-butylhydrazine hydrochloride into a reaction container filled with a stirring device, stirring for 10-30 minutes, cooling to the temperature of 0-4 DEG C, and adding ferric trichloride; reacting at the temperature of 0-4 DEG C for 1-3 hours, immediately filtering after the reaction is ended, washing the filter cake with a small amount of cold ethanol, and drying, namely obtaining the product. The process disclosed by the invention is simple, and the purity of the tert-butylhydrazine hydrochloride is greatly improved. Moreover,less three wastes are produced in the production process, the environmental protection is facilitated, and the process is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of pesticides and pesticide intermediates. Background technique [0002] Tert-Butylhydrazine Hydrochloride (Tert-Butylhydrazine Hydrochloride), also known as Tert-Butylhydrazine Hydrochloride, is an important pesticide intermediate. It is an important raw material for the synthesis of insecticides such as hydrazine, tebufenozide, chlorfenozide, methoxyfenozide, cyclofenozide and pyridaben. [0003] At present, the purity of tert-butylhydrazine hydrochloride obtained in industrial production is about 90%. The main impurity is hydrazine hydrochloride. The existence of hydrazine hydrochloride leads to waste of raw materials in the production of downstream products; introduces new impurities in downstream products; increases the difficulty of purification of downstream products. [0004] Since the solubility of tert-butylhydrazine hydrochloride in water is relatively large, and the solubility does not change significan...

Claims

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Application Information

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IPC IPC(8): C07C243/14C07C241/02
CPCC07C241/02C07C243/14
Inventor 刘立业赵文卓史晋宜丁元生
Owner JILIN INST OF CHEM TECH
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