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A kind of preparation method of high purity and low water content 3-methylamine tetrahydrofuran

A technology of methylamine tetrahydrofuran and water content, applied in the direction of organic chemistry, can solve problems such as low conversion rate, high production cost, and product purity to be improved, achieve high amination rate, reduce by-product formation, and improve product quality The effect of purity

Active Publication Date: 2020-04-28
ZHEJIANG XIANFENG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] This invention application provides a synthesis method of 3-methylamine tetrahydrofuran, but the purity of the product obtained by the synthesis method still needs to be improved, and the conversion rate of the reaction is low, which leads to higher production costs

Method used

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  • A kind of preparation method of high purity and low water content 3-methylamine tetrahydrofuran
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  • A kind of preparation method of high purity and low water content 3-methylamine tetrahydrofuran

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Embodiment 1

[0030] Such as figure 1 As shown, the present embodiment provides a method for preparing high-purity and low-water-content 3-methylamine tetrahydrofuran, specifically, comprising the following steps:

[0031] Step 1: Add anhydrous methanol into the reaction kettle, stir and cool, then add 1.2 parts of liquid ammonia and 1 part of 3-formaldehyde tetrahydrofuran in sequence, and stir and react under nitrogen protection to obtain sub For amine intermediates, the temperature of the reaction system should not exceed 0°C during the entire process from the addition of anhydrous methanol to the completion of the reaction;

[0032] Step 2: Add palladium carbon with a mass fraction of 0.1 part and the imine intermediate prepared in step 1 into the reaction kettle, protect it with nitrogen, stir and heat up to 35°C, and feed hydrogen gas so that the hydrogen pressure in the kettle is 1.0 MPa, continue to heat up to 65°C for 3h;

[0033] Step 3: cooling, the reaction solution is filtere...

Embodiment 2

[0038] Such as figure 1 As shown, the present embodiment provides a method for preparing high-purity and low-water-content 3-methylamine tetrahydrofuran, specifically, comprising the following steps:

[0039] Step 1: Add anhydrous methanol into the reaction kettle, stir and cool, then add 1.5 parts of liquid ammonia and 1 part of 3-formaldehyde tetrahydrofuran in sequence, and stir and react under nitrogen protection to obtain sub For amine intermediates, the temperature of the reaction system should not exceed 0°C during the entire process from the addition of anhydrous methanol to the completion of the reaction;

[0040] Step 2: Add Raney nickel with a mass fraction of 0.03 parts and the imine intermediate prepared in step 1 into the reaction kettle, protect it with nitrogen, stir and heat up to 40°C, and feed hydrogen gas so that the hydrogen pressure in the kettle is 2.0MPa, continue to heat up to 75°C for 5h;

[0041] Step 3: lowering the temperature, filtering the reac...

Embodiment 3

[0044] Such as figure 1 As shown, the present embodiment provides a method for preparing high-purity and low-water-content 3-methylamine tetrahydrofuran, specifically, comprising the following steps:

[0045] Step 1: Add anhydrous methanol into the reaction kettle, stir and cool, then add 1.35 parts of liquid ammonia and 1 part of 3-formaldehyde tetrahydrofuran in sequence, and stir the reaction under nitrogen protection to obtain sub For amine intermediates, the temperature of the reaction system should not exceed 0°C during the entire process from the addition of anhydrous methanol to the completion of the reaction;

[0046] Step 2: Add Raney nickel with a mass fraction of 0.05 parts and the imine intermediate prepared in step 1 into the reaction kettle, protect it with nitrogen, stir and heat up to 38°C, and feed hydrogen gas so that the hydrogen pressure in the kettle is 1.5MPa, continue to heat up to 70°C for 4h;

[0047] Step 3: lowering the temperature, filtering the ...

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Abstract

The invention discloses a preparation method of 3-methylamine tetrahydrofuran with high purity and low water content. The preparation method comprises the following steps: (1) reacting liquid ammoniawith 3-methanal tetrahydrofuran in the presence of absolute methanol to obtain an imine intermediate; and (2) in the presence of a catalyst, reacting the imine intermediate with hydrogen, cooling after the reaction is finished, filtering a reaction liquid to remove the catalyst, then transferring the solution into a distillation still, distilling and recycling ammonia gas and methyl alcohol, thenheating for distillation, and collecting fractions to obtain 3-methylamine tetrahydrofuran, wherein the internal temperature of the still is 75 to 80 DEG C, and the top temperature of the still is 65to 75 DEG C. Compared with the prior art, the prepared 3-methylamine tetrahydrofuran has higher purity and lower water content, the intermediate with high quality is provided for further synthesis ofother chemical products by using methanal tetrahydrofuran, the raw materials are also recycled, the production cost is reduced, the preparation method is energy-saving and environmentally-friendly, and the preparation method accords with current idea of green chemistry.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a preparation method of high-purity and low-water content 3-methylamine tetrahydrofuran. Background technique [0002] 3-Methylamine tetrahydrofuran is an important intermediate for the synthesis of the third-generation nicotinic insecticide dinotefuran and other new drugs. Dinotefuran was developed by Mitsui Corporation of Japan and was first registered and listed in Japan in 2002. Now it is in Pesticide registrations have been obtained in several countries. Due to its special structure, compared with traditional neonicotinoid insecticides, dinotefuran has better performance, has excellent systemic penetration, and shows high insecticidal activity at a very low dose. Therefore, dinotefuran is safe to animals and plants, has a long residual effect, and has a broad spectrum of insecticidal properties. It is suitable for rice, vegetables, fruit trees and flowers to control...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/14
CPCC07D307/14
Inventor 高军龙陈小平高飞飞李明朱敏亮
Owner ZHEJIANG XIANFENG TECH