An improved process for synthesizing n-(6-chloro-3-pyridylmethyl)-methylamine
A technology of picolylmethyl and chloromethylpyridinetoluene, which is applied in the field of improved technology for synthesizing N-methylamine, can solve the problems of increasing the consumption of raw material methylamine, increasing the amount of waste water produced, increasing environmental protection treatment, etc., achieving reduction The effect of waste water production, reduction of pollutant discharge, and improvement of equipment utilization efficiency
Active Publication Date: 2016-08-10
安徽新北卡化学有限公司
View PDF4 Cites 0 Cited by
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
The use of 30% monomethylamine aqueous solution in the above reaction process not only increases the amount of waste water produced, but also increases the difficulty of subsequent environmental protection treatment. At the same time, all the hydrogen chloride gas generated in the reaction process will be dissolved in the same methylamine The reaction occurs, which not only increases the consumption of the raw material monomethylamine, but also increases the by-products, resulting in high production costs
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View moreImage
Smart Image Click on the blue labels to locate them in the text.
Smart ImageViewing Examples
Examples
Experimental program
Comparison scheme
Effect test
Embodiment Construction
[0022] The following examples further illustrate the present invention, but do not limit the present invention.
[0023] An improved technique for synthesizing N-(6-chloro-3-pyridylmethyl)-methylamine, the concrete steps are as follows:
[0024] (1) at first add 1400kg toluene in the 3000L glass-lined reactor reactor, then cool the reaction system, when the temperature drops to -5 ℃~5 ℃, feed 250kg monomethylamine gas to make it completely dissolved in toluene , the gas introduction speed of monomethylamine is about 100~200kg / h;
[0025] (2) 500kg 2-chloro-5-chloromethyl pyridine is dissolved in 150kg toluene, after stirring, obtain 2-chloro-5-chloromethyl pyridine toluene solution, it is added dropwise in the reactor, keep stirring state, The dropwise addition time is about 5 hours, and the reaction temperature is kept in the range of -5°C-2°C;
[0026] (3) after dripping finishes, feed monomethylamine gas 200kg into the reactor again, the monomethylamine gas feed speed is ...
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More PUM
Login to View More Abstract
The invention discloses an improved process for synthesizing N-(6-chloro-3-picolyl)-methylamine. The improved process comprises the following steps of: adding toluene and monomethyl amine gases into a reaction kettle; cooling to 5 DEG C below zero to 5 DEG C; dropwise adding a 2-chloro-5-chloromethylpyridinetoluene solution to generate N-(6-chloro-3-picolyl)-methylamine; washing with water and delaminating; and removing toluene from an oil layer by distilling to obtained refined N-(6-chloro-3-picolyl)-methylamine. The method disclosed by the invention has the advantages of reduction in raw material using amount, reduction in transportation cost, environment-friendly synthesis process, small amount of produced waste water, high product purity and suitability for industrial production.
Description
technical field [0001] The invention relates to the field of fine chemicals, in particular to an improved process for synthesizing N-(6-chloro-3-pyridylmethyl)-methylamine. Background technique [0002] N-(6-chloro-3-pyridylmethyl)-methylamine is an important intermediate for the preparation of insecticides imidacloprid and acetamiprid. The name of N-(6-chloro-3-pyridylmethyl)-methylamine can be found in "Synthesis of Insecticide Acetamiprid" by Sun Yuquan, Journal of Weifang Institute of Education, No. 2, 2006. At present, the synthetic method adopted by factories in my country is: Toluene and 30% monomethylamine aqueous solution were added to the reactor, cooled to -5℃~5℃, 2-chloro-5-chloromethylpyridine toluene solution was added dropwise to generate N-(6-chloro-3-pyridine methyl)-methylamine, washed with water, layered, and the oil layer was distilled to remove toluene to obtain N-(6-chloro-3-pyridylmethyl)-methylamine. The above reaction process uses the use of 30% mono...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More Application Information
Patent Timeline
Login to View More Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/61
Inventor 陈前虎
Owner 安徽新北卡化学有限公司