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A kind of synthetic technique of increasing production amine

A synthesis process and a technology for increasing the production of amines, which are applied in the field of preparation technology for increasing the production of amines, can solve the problems of long preparation time, short synthesis time, and low cost of the production-increasing amines, and achieve shortening of reaction time, improvement of solvent recovery rate, and elimination of reaction inhibition Effect

Active Publication Date: 2018-04-13
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0017] The present invention aims to solve the problems of long preparation time, low yield and high cost of production-increasing amines in the prior art, and provides a new synthesis process for production-increasing amines, replacing the heterogeneous reaction in the prior art with a homogeneous reaction, There is no need to add a phase transfer catalyst, which has the advantages of short synthesis time, low cost and high yield of final product

Method used

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  • A kind of synthetic technique of increasing production amine
  • A kind of synthetic technique of increasing production amine
  • A kind of synthetic technique of increasing production amine

Examples

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Effect test

Embodiment 1

[0045] A kind of synthetic technique of increasing production amine, comprises the following steps:

[0046]A. After dissolving 3,4-dichlorophenol and alkali metal hydroxide in a polar aprotic solvent, add 1,2-dihaloethane, heat up, keep warm and reflux for 0.5h, rectify, and recover untreated The reacted 1,2-dihaloethane and some polar aprotic solvents, the bottom of the still is a mixture of intermediate products and polar aprotic solvents;

[0047] B. Add diethylamine to the mixed solution of the intermediate product obtained in step A and the polar aprotic solvent, heat to reflux for 8 hours, then add alkali metal hydroxide, stir, then filter, and obtain after rectification of the filtrate Increase production of amine;

[0048] In the above step A and step B, the alkali metal hydroxide is potassium hydroxide.

Embodiment 2

[0050] A synthesis technique for increasing production of amines, comprising the following steps:

[0051] A. After dissolving 3,4-dichlorophenol and alkali metal hydroxide in a polar aprotic solvent, add 1,2-dihaloethane, heat up, keep warm and reflux for 1 hour, rectify, and recover unreacted 1,2-dihaloethane and some polar aprotic solvents, the bottom of the still is a mixed solution of intermediate products and polar aprotic solvents;

[0052] B. Add diethylamine to the mixture of the intermediate product obtained in step A and the polar aprotic solvent, heat to reflux for 10 hours, then add alkali metal hydroxide, stir, then filter, and obtain Increase production of amine;

[0053] In the above step A and step B, the alkali metal hydroxide is sodium hydroxide.

[0054] The polar aprotic solvent in this example is DMF; in step A, the 1,2-dihaloethane is 1,2-dichloroethane.

Embodiment 3

[0056] A synthesis technique for increasing production of amines, comprising the following steps:

[0057] A. After dissolving 3,4-dichlorophenol and alkali metal hydroxide in a polar aprotic solvent, add 1,2-dihaloethane, heat up, keep warm and reflux for 0.5h, rectify, and recover untreated The reacted 1,2-dihaloethane and some polar aprotic solvents, the bottom of the still is a mixture of intermediate products and polar aprotic solvents;

[0058] B. Add diethylamine to the mixture of the intermediate product obtained in step A and the polar aprotic solvent, heat to reflux for 9 hours, then add alkali metal hydroxide, stir, then filter, and obtain after rectification of the filtrate Increase production of amine;

[0059] In the above step A and step B, the alkali metal hydroxide is sodium hydroxide.

[0060] The polar aprotic solvent in this example is DMAC; in step A, the 1,2-dihaloethane is 1,2-dibromoethane; the amount of alkali metal hydroxide is 3,4-di The amount of...

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Abstract

The invention discloses a synthetic process of DCPTA [2-(3,4-dichlorophenoxy)trithylamine] and belongs to the technical field of fine chemicals. The process comprises the following steps: A, 3,4-Dichlorophenol and alkali metal hydroxide are dissolved into a polar aprotic solvent, 1,2-dihaloethane is added, thermal insulation backflow is performed for 0.5 to 1 hour, rectifying is performed, unreacted 1,2-dihaloethane and part of polar aprotic solvent are recycled, and a mixed liquor of intermediate products and the polar aprotic solvent is left on a kettle bottom; B, diethylamine is added into the mixed liquor of the intermediate products and the polar aprotic solvent, obtained in the step A, after thermal insulation backflow lasts for 8 to 10 hours, alkali metal hydroxide is added, stirring is performed, then filtering is performed, and after the rectification of the filter liquor, the DCPTA is obtained. In the synthetic process provided by the invention, by changing the traditional heterogeneous reaction to be a homogeneous reaction, the cost is lowered, side reactions are controlled, and the product yield is improved.

Description

technical field [0001] The invention relates to a preparation process of production-increasing amine, which belongs to the technical field of fine chemicals. Background technique [0002] Yield-increasing amine, chemical name 2-(3,4-dichlorophenoxy)ethyldiethylamine, is a new type of plant growth regulator discovered by Yokoyama et al. in 1977 and developed by American Stauffer Company. By promoting, increasing or inhibiting, reducing the level of endogenous plant hormones, it can effectively regulate the growth and development of plants. It has different degrees of yield-increasing effect on crops such as soybean, corn, wheat, cotton, sugar beet, ginseng guayule and various vegetables. It can be used in combination with a variety of pesticides and fertilizers to enhance the disease resistance of plants and improve the bactericidal effect. Yield-increasing amines are widely used in agriculture because of their unique multifunctional effects. [0003] The synthesis methods...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/20C07C213/02
CPCC07C41/16C07C213/02C07C217/20C07C43/225
Inventor 罗茜彭舟李舟张华王蕾张蕾
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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