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Preparation method of tert-butylhydrazine hydrochloride

A technology for tert-butylhydrazine and hydrochloride, which is applied in the field of preparation of tert-butylhydrazine hydrochloride, can solve the problems of low utilization rate of raw materials, high discharge of three wastes, low product yield, etc., and achieves easy control of reaction , avoid side reactions, improve the effect of raw material utilization

Inactive Publication Date: 2018-09-25
SHANGHAI SHISI CHEM PROD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The problem to be solved by the present invention is to provide a preparation method of tert-butylhydrazine hydrochloride, to overcome the low utilization rate of raw materials in the preparation process of tert-butylhydrazine hydrochloride in the prior art, low product yield, and three waste discharges High disadvantage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The present embodiment provides a kind of preparation method of tert-butylhydrazine hydrochloride, concrete implementation is as follows:

[0025] Add 100g of hydrazine hydrate (content 32%) (1.0mol) into a 500ML three-neck flask equipped with a thermometer, dropping funnel, stirring, and water separator, acidify with formic acid to pH ≈ 2 at room temperature, record and calculate the dosage, and heat the inner temperature to 40-50°C, stirred and reacted for 30 minutes, added 1.5mol 111g of tert-butanol dropwise to the reaction solution, and the dropwise addition was completed in 60 minutes, then heated up and refluxed for 6 hours, cooled to room temperature, and acidified with 1.5mol hydrogen chloride while stirring, and again Heat up and reduce pressure to distill out water, formic acid, excess tert-butanol and other low-boiling substances. Rinse the solid with 300ml of methanol, collect the eluate, weigh, and dry the solid at 120°C to obtain 111.2 g of tert-butylhydr...

Embodiment 2

[0027] Add 150g of hydrazine salt solution (content 32%) (1.5mol) into a 500ML three-necked flask equipped with a thermometer, dropping funnel, stirring, and water separator, acidify with acetic acid to pH ≈ 3 at room temperature, record and calculate the dosage, and heat the Warm to 40-50°C, stir and react for 30 minutes, add 1.95mol 144.3g tert-butanol dropwise to the reaction liquid, dropwise complete in 90 minutes, heat up and reflux for 7 hours, cool to room temperature, and pass 2.0mol hydrogen chloride into the reaction solution to acidify , Heating again under reduced pressure to distill water, acetic acid, excess tert-butanol and other low boiling point substances. Rinse the solid with 400ml of ethanol, collect the eluate, weigh, and dry the solid at 120°C to obtain 160.3g of tert-butylhydrazine hydrochloride white solid, the content of tert-butylhydrazine hydrochloride is 98.3% (HPLC), and the yield is 85.8% %.

Embodiment 3

[0029] Add 100g of hydrazine salt solution (48% content) (1.5mol) into a 500ML three-necked flask equipped with a thermometer, dropping funnel, stirring, and water separator, acidify with acetic acid to pH ≈ 3 at room temperature, record the calculated dosage, and heat the Warm to 40-50°C, stir and react for 30 minutes, add 2.25mol 166.5g of tert-butanol dropwise to the reaction liquid, dropwise complete in 90 minutes, heat up to reflux for 6 hours, cool to room temperature, pass 3mol hydrogen chloride into the reaction solution for acidification, The temperature was raised and the low boiling point substances such as water, acetic acid and excess tert-butanol were distilled under reduced pressure again. Rinse the solid with 400ml of ethanol, collect the eluent, weigh, and dry the solid at 120°C to obtain 166.3g of tert-butylhydrazine hydrochloride white solid, tert-butylhydrazine hydrochloride content 99.1% (HPLC), yield 89.1 %.

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Abstract

The invention discloses a preparation method of tert-butylhydrazine hydrochloride. According to the preparation method, tert-butyl alcohol and hydrazine hydrate are used as initial raw materials, andan organic acid buffering solution system is used for preparing a tert-butylhydrazine-organic acid solution; then hydrogen chloride is used for carrying out acidification reaction to prepare the tert-butylhydrazine hydrochloride. Compared with the prior art, the method abolishes a step of carrying out acidification by directly utilizing hydrochloric acid or hydrogen chloride gas in a process of synthesizing tert-butylhydrazine and side reactions including tert-butyl alcohol dehydration and the like are reduced; the reaction is mild and easy to control. The total yield of the reaction can reach85 percent or more, and the wastewater amount and the VOC (Volatile Organic Compound) emission amount are greatly reduced; the preparation method meets the requirements of green chemical industry andis suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method for preparing tert-butylhydrazine hydrochloride. Background technique [0002] Tert-butylhydrazine hydrochloride is an important pesticide intermediate, which can be used to synthesize benzoylhydrazine insecticides, dihydrazide insecticides, tebufenozide (tebufenozide), chlorantranilis Halofenozide, methoxyfenozide, and chromafenozide, and the acaricide pyridaben. At the same time, it can also be used as a raw material for synthetic medicine and materials. [0003] In the prior art, hydrochloric acid is generally used to acidify hydrazine hydrate, and then react with tert-butanol to directly react to prepare tert-butylhydrazine hydrochloride. But the yield of this method is low, the main reason is that in the reaction process of tert-butanol and hydrazine hydrate hydrochloride, the acidity of hydrochloric acid is too strong to cause the dehydration reaction of tert-butanol to produce olefinic compounds, i...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/14
CPCC07C241/02C07C243/14
Inventor 张传好周龙达李海涛
Owner SHANGHAI SHISI CHEM PROD
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