1-(4-morpholinylphenyl)-1-butanone preparation method

A technology of morpholine phenyl and methyl ethyl ketone, which is applied in the field of preparation of α-aminoacetophenone-based photoinitiator intermediates, can solve the problems of cumbersome post-processing, long reaction time, and dangerous addition of materials, so as to reduce the risk of reaction, The effect of shortening the response cycle and reducing risks

Active Publication Date: 2019-05-07
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] First of all, 1-(4-chlorophenyl)-1-butanone has a safety hazard in the reaction process, so its accumulation should be properly controlled
There are two ways to control the accumulation of 1-(4-chlorophenyl)-1-butanone, one is to add continuously for a long time under the reaction temperature and pressure; the other is to use a catalyst such as cuprous chloride to accelerate the reaction to a certain extent; The former has a long reaction time and is dangerous to feed under high temperature and high pressure, and has higher requirements on the reac

Method used

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Embodiment 1

[0025] Embodiment 1: Preparation of 1-(4-morpholine phenyl)-1-butanone

[0026] Dissolve morpholine (336.5g, 4.0mol) in water (360.0g, 20.0mol), then add 1-(4-chlorophenyl)-1-butanone (182.7, 1.0mol), and stir well, Put it into a 1.5L high-pressure reactor, close the reactor, and heat the reaction solution to 210-215°C within 1.5-2 hours, while the pressure in the reactor is also rising, control the pressure in the reactor at about 20bar, and keep warm for 8 hours Then cool down and crystallize, shake off the filter, wash the filter cake with water, and dry to obtain 222.8 g of beige crystals with a purity of 99.1% and a melting point of 65.5-66.5°C.

[0027] After centrifugation, the filtrate was collected for morpholine recovery, and 40.0 g of sodium hydroxide was added under stirring. After the addition, all fractions of the morpholine and water mixture were collected by heating distillation, and directly applied mechanically.

Embodiment 2

[0028] Embodiment 2: Preparation of 1-(4-morpholine phenyl)-1-butanone

[0029] Dissolve morpholine (261.0g, 3.0mol) in water (360.0g, 20.0mol), then add 1-(4-chlorophenyl)-1-butanone (182.7, 1.0mol), and stir well, Put it into a 1.5L high-pressure reactor, close the reactor, and heat the reaction solution to 210-215°C within 1.5-2 hours, while the pressure in the reactor is also rising, control the pressure in the reactor at about 20bar, and keep warm for 10 hours Then cool down and crystallize, shake off the filter, wash the filter cake with water, and dry to obtain 220.8 g of beige crystals with a purity of 99.3% and a melting point of 65.5-66.5°C.

Embodiment 3

[0030] Example 3: Preparation of 1-(4-morpholine phenyl)-1-butanone

[0031] Dissolve morpholine (217.5g, 2.5mol) in water (360.0g, 20.0mol), then add 1-(4-chlorophenyl)-1-butanone (182.7, 1.0mol), and stir well, Put it into a 1.5L high-pressure reactor, close the reactor, and heat the reaction liquid to 210-215°C within 1.5-2 hours, while the pressure in the reactor is also rising, control the pressure in the reactor at about 20bar, and keep warm for 28 hours Then cool down and crystallize, shake off the filter, wash the filter cake with water, and dry to obtain 186.0 g of beige crystals with a purity of 93.5%.

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Abstract

The invention relates to an alpha-aminoacetophenone photoinitiator intermediate preparation method, particularly to a preparation method of an intermediate of photoinitiators 2-benzyl-2-dimethylamino-1-(4-morpholinylphenyl)butanone and 2-(4-methylbenzyl)-2-dimethylamino-1-(4-morpholinylphenyl)butanone. According to the present invention, the disadvantages in the prior art are overcome, and the alpha-aminoacetophenone photoinitiator intermediate preparation method is provided, wherein the method does not require high-temperature and high-pressure feeding, has simple post-treatment, has good product appearance, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of an α-aminoacetophenone photoinitiator intermediate, in particular to a photoinitiator 2-benzyl-2-dimethylamino-1-(4-morpholine phenyl) butanone and the preparation method of 2-(4-methylbenzyl)-2-dimethylamino-1-(4-morpholine phenyl) butanone intermediate 1-(4-morpholine phenyl)-1-butanone . Background technique [0002] α-aminoketone photoinitiator is a class of important photoinitiator, in which 2-benzyl-2-dimethylamino-1-(4-morpholine phenyl) butanone and 2-(4-methyl Benzyl)-2-dimethylamino-1-(4-morpholine phenyl) butanone is an α-aminoketone photoinitiator developed by Ciba Company, and its trade names are "Irgacure 369" and "Irgacure 379" respectively , this kind of photoinitiator has good thermal stability, long storage period, good solubility, light color, good anti-yellowing performance, fast photocuring speed, and good deep curing performance, especially used in colored systems, in the field of...

Claims

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Application Information

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IPC IPC(8): C07D295/112
Inventor 罗想武瑞王涛毛桂红张齐
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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