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Preparation method of hydrazide compound

A compound and hydrazide technology, applied in the field of preparation of hydrazide compounds, can solve the problems of explosion, environmental pollution, strong reducibility, etc., and achieve the effects of small safety risk, wide application range and improved production efficiency

Active Publication Date: 2013-11-27
LANZHOU UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hydrazine hydrate is a highly reducing, explosive, and toxic compound, and its large-scale use in industrial production has a greater risk and causes environmental pollution

Method used

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  • Preparation method of hydrazide compound
  • Preparation method of hydrazide compound
  • Preparation method of hydrazide compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 Synthesis of butanoic acid, hydrazide, CAS: 3538-65-6

[0041] Add 116g of ethyl butyrate and 75g of 80% hydrazine hydrate into a three-necked flask equipped with a magnet, and install a thermometer and a rectifying column. Heat the three-neck flask and start stirring, and reflux for half an hour. When the temperature at the top of the rectifying column reaches 80°C, the by-products ethanol and water will distill out. Control the temperature of the reaction system at 82-101°C, and the temperature at the top of the rectifying column at 75-85°C. After 6 hours of reaction, the reaction was completed, and the heating was stopped and stirred. After the reaction was completed, vacuum distillation was performed to distill off excess hydrazine hydrate, water, and a small amount of ethyl butyrate to obtain 93.8 g of hydrazine butyrate product, with a yield of 92%. 1 H NMR (400MHz, CDCl 3 , δ, ppm): 0.94-0.99 (t, 3H, CH 3 ), 1.64-1.74 (sextet, 2H, CH 2 ), 2.12-2.22 (...

Embodiment 2

[0042] Example 2 Synthesis of hydrazine pentanoate (Pentanohydrazide, CAS: 38291-82-6)

[0043] Add 130g of ethyl valerate and 75g of 80% hydrazine hydrate into a three-necked flask equipped with a magnet, and install a thermometer and a rectifying column. Heat the three-neck flask and start stirring, and reflux for half an hour. When the temperature at the top of the rectifying column reaches 80°C, the by-products ethanol and water will distill out. Control the temperature of the reaction system at 85-105°C, and the temperature at the top of the rectification column at 75-85°C. After 6 hours of reaction, the reaction was completed, and the heating was stopped and stirred. After the reaction was completed, vacuum distillation was performed to distill off excess hydrazine hydrate, water, and a small amount of ethyl valerate to obtain 106.7 g of hydrazine valerate, with a yield of 92%. 1 H NMR (400MHz, CDCl 3 , δ, ppm): 0.90-0.94 (t, 3H, CH 3 ), 1.31-1.40 (sextet, 2H, CH 2 ...

Embodiment 3

[0044] Example 3 Synthesis of Heptanohydrazide (CAS: 22371-32-0)

[0045] Add 158 g of ethyl heptanoate and 75 g of 80% hydrazine hydrate into a three-necked flask equipped with a magnet, and install a thermometer and a rectifying column. Heat the three-neck flask and start stirring, and reflux for half an hour. When the temperature at the top of the rectifying column reaches 80°C, the by-products ethanol and water will distill out. Control the temperature of the reaction system at 88-112°C, and the temperature at the top of the rectifying column at 75-85°C. After 6 hours of reaction, the reaction was completed, and the heating was stopped and stirred. After the reaction was completed, vacuum distillation was performed to distill off excess hydrazine hydrate, water, and a small amount of ethyl heptanoate to obtain 133.92 g of heptanyl hydrazide product, with a yield of 93%. 1 H NMR (400MHz, CDCl 3 , δ, ppm): 0.87-0.92(t, 3H, CH 3 ), 1.30-1.32(t, 6H, 3CH 2 ), 1.62-1.69 (m,...

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Abstract

The invention discloses a preparation method of a hydrazide compound. The preparation method comprises the following steps of adding an ester and hydrazine hydrate into a reactor, carrying out heating reflux for 0.5-2h, carrying out reaction fractionation or reaction rectification, wherein by control, the distillates comprise an alcohol compound and water, and after the reaction, carrying out reduced pressure distillation to obtain the hydrazide compound. The preparation method has a high raw material utilization rate, does not produce waste, does not utilize a reaction solvent, improves reactor volume use efficiency, improves production efficiency, has simple processes, has a hydrazide compound yield more than 90%, realizes ton-magnitude hydrazide industrial production, has a small safety risk and has a wide substrate application range.

Description

technical field [0001] The invention relates to a method for preparing hydrazide compounds, which is an improvement on the existing method for preparing hydrazide compounds. Background technique [0002] Hydrazide compounds are very important fine chemicals. Hydrazide compounds are widely used. For example, in the field of medicine, aromatic hydrazide compounds are used to prepare immunosuppressants; Formaldehyde adsorbent; in the field of agricultural science, bishydrazide compounds can also be used as pest inhibitors to inhibit the reproduction of pests. In addition, hydrazide compounds are also an important class of organic synthesis intermediates. [0003] At present, according to literature reports, the synthesis of hydrazide compounds mainly contains the following four methods: [0004] Method one acid chloride hydrazinolysis: This method uses acid chloride and hydrazine hydrate to prepare hydrazide through nitrogen acylation in the presence of alkali. In this metho...

Claims

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Application Information

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IPC IPC(8): C07C241/04C07C243/28
CPCY02P20/10
Inventor 许鹏飞曹建胡秀琴罗永春王瑶徐国强
Owner LANZHOU UNIVERSITY
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