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Preparation method of 2-methyl-2-(4-morpholinyl)-1-[4-(methylthio)phenyl]-1-acetone

A technology of methylthio and morpholino, which is applied in the field of preparation of 2-methyl-2-(4-morpholinyl)-1-[4-(methylthio)phenyl]-1-acetone, It can solve the problems of low yield and unfriendly smell of the final product, and achieve the effects of high purity, low cost and simple process equipment.

Active Publication Date: 2013-09-25
湖南久日新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This process also has problems such as low yield and unfriendly odor of the final product

Method used

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  • Preparation method of 2-methyl-2-(4-morpholinyl)-1-[4-(methylthio)phenyl]-1-acetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: the preparation of 2-chloro-2-methylpropionyl chloride

[0022] Mix 30g (0.34mol) of isobutyric acid and 26g (0.17mol) of phosphorus oxychloride, and heat to 75°C for 1.5h. Chlorine gas was introduced into the reaction solution and stirred for 20h. Distilled under reduced pressure (pressure 20KPa) to obtain 43.2 g of 2-chloro-2-methylpropionyl chloride. Yield: 90%, content 97%.

[0023] Boiling point: 90-91°C (pressure 20KPa).

[0024] 1 HNMR (CDCl 3 ): δ1.60(s, 6H).

Embodiment 2

[0025] Embodiment 2: Preparation of 2-chloro-2-methylpropionyl chloride

[0026] Mix 30g (0.34mol) of isobutyric acid and 23.4g (0.17mol) of phosphorus trichloride, and heat to 70°C for 1.5h. Chlorine gas was introduced into the reaction solution and stirred for 20h. Distilled under reduced pressure (pressure 20KPa) to obtain 41.2 g of 2-chloro-2-methylpropionyl chloride. Yield: 86%, content: 97%.

Embodiment 3

[0027] Example 3: Preparation of 2-methyl-2-chloro-1-[4-(methylthio)phenyl]-1-propanone

[0028] Cool 120mL of dichloromethane to 5°C with an ice-water bath, add 16.8g (0.126mol) of aluminum trichloride, slowly add 16.0g (0.113mol) of 2-chloro-2-methylpropionyl chloride for 20min, and slowly add 11.3 g (0.091mol) sulfide anisole for 30min. Heated to 50°C and stirred for 1.5h. The reaction liquid was cooled to 20°C, added into 120 mL of 10% industrial hydrochloric acid and stirred for 1 h. Let stand, separate the water layer, wash the organic phase with water until neutral, and dry with anhydrous sodium sulfate for 10 h. Precipitation under low pressure gave 17.5 g of light yellow oily substance, namely 2-methyl-2-chloro-1-[4-(methylthio)phenyl]-1-propanone. Yield: 85%, content: 95%.

[0029] 1 H NMR (CDCl 3 ) δ 1.62 (s, 6H), 2.47 (s, 3H), 7.22 (d, 2H), 7.79 (d, 2H).

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Abstract

The invention a preparation method of 2-methyl-2-(4-morpholinyl)-1-[4-(methylthio)phenyl]-1-acetone. The 2-methyl-2-(4-morpholinyl)-1-[4-(methylthio)phenyl]-1-acetone prepared by the method provided by the invention is an efficient radical ultraviolet initialtor and is suitable for the single-function or multifunctional monomer ultraviolet curing system and an acrylate prepolymer. The compound can be used alone or used together with photo initiators (ITX and 184). As the compound has efficient ultraviolet absorption property, the compound is especially suitable for being used in the formulas of oil and colored paint such as offset ink, silk screen printing ink and printing plate-making photoresist. The method has the advantages of simple processing equipment, easiness for operation and low cost; the prepared compound has high purity; and the product purity reaches more than 99%.

Description

technical field [0001] The invention relates to a preparation method of high-efficiency free radical photoinitiator 2-methyl-2-(4-morpholinyl)-1-[4-(methylthio)phenyl]-1-propanone. Background technique [0002] 2-Methyl-2-(4-morpholinyl)-1-[4-(methylthio)phenyl]-1-propanone is a high-efficiency UV photoinitiator, suitable for single and multifunctional monomer UV Light-curing systems and acrylate prepolymers. At present, there are mainly five methods for synthesizing this compound. The Ciba-Geigy company patent EP0088050 reports that sulfide anisole is used as a raw material, and the obtained methylthio isobutyl ketone is brominated, and the target product is obtained through the ring-opening reaction of an epoxy intermediate and morpholine. The patent CN1354175A of Beijing Yingli High Technology Development Co., Ltd. reported that sulfide anisole was used as a raw material, and the obtained methylthio isobutyl ketone was brominated, and reacted with morpholine in the pres...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/104
Inventor 赵国锋罗想张齐毛桂红郑勇王昆杨天艳李晓娟李欢欢
Owner 湖南久日新材料有限公司
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