Preparation method of 2-methyl-1-(4-substituted phenyl)-2-morpholinyl-1-acetone

Abstract

The invention relates to a preparation method of 2-methyl-1-(4-substituted phenyl)-2-morpholinyl-1-acetone. The preparation method comprises two steps of epoxidation reaction and morpholine substitution reaction, wherein in the morpholine substitution reaction, a proper amount of an auxiliary agent is added, and the auxiliary agent is selected from at least one of water, a strong-acid weak-alkalisaline solution and a strong-alkali weak-acid saline solution, so that the ring opening rate and the ring opening selectivity in the morpholine substitution reaction process can be obviously improved,and the overall reaction rate and yield are further improved, according to the method, the problem that subsequent catalysts are difficult to filter, recycle and purify due to the fact that catalystssuch as carclazyte need to be added in the traditional process is solved, the high-purity 2-methyl-1-(4-substituted phenyl)-2-morpholinyl-1-acetone can be obtained more easily, the process cost and the aftertreatment operation risk are reduced, and the economic benefit is improved.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a preparation method of 2-methyl-1-(4-substituted phenyl)-2-morpholino-1-propanone, in particular to a high-purity 2-methyl-1-propanone The preparation method of 1-(4-substituted phenyl)-2-morpholino-1-propanone. Background technique [0002] 2-methyl-1-(4-methylthiophenyl)-2-morpholino-1-propanone (ultraviolet photoinitiator 907) can absorb ultraviolet radiation energy to form free radicals or Cationic, triggering the polymerization, crosslinking and grafting reactions of monomers and oligomers, and curing the ink into a three-dimensional network structure polymer in a short time; the molecular structure of UV photoinitiator 907 is as follows : [0003] [0004] Regarding the synthetic method of ultraviolet photoinitiator 907, CN101633647A discloses a method for synthesizing α-aminoaryl alkyl ketones with high selectivity and high yield. The synthetic method consists of Fried...

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Problems solved by technology

[0004] Regarding the synthetic method of ultraviolet photoinitiator 907, CN101633647A discloses a method for synthesizing α-aminoaryl alkyl ketones with high selectivity and high yield. The synthetic method consists of Friedel-Crafts reaction, bromination reaction, epoxidation Reaction and amine substitution ring-opening reaction composition, and add catalyst when epoxide reacts with organic amine, described catalyst is obtained with any one or more in montmorillonite, kaolin, clay, bentonite or white clay; The synthesis method has the problem of difficult separation of the catalyst after the subsequent ring-opening reaction, high operating costs, and the product produced by the reaction is dark in color, and 5-10% activated carbon is required for decolorization

[0005] CN102659717A discloses a synthetic method of 2-methyl-1-(4-methylthiophenyl)-2-morpholino-1-acetone, in which the ring-opening process is acidified with hydrochloric acid to obtain 1-(4-chloro Phenyl)-2-methyl-2-morpholinyl-1-propanol hydrochloride, followed by oxidation and substitution to obtain the target product 2-methyl-1-(4-methylthiophenyl)-2 -Morpholinyl-1-acetone; this synthetic method increases the oxidation step, the process is complicated, and the cost is high

CN110563671A discloses a kind of preparation method of photoinitiator 2-methyl-1-(4-methylthiophenyl)-2-morpholino-1-acetone, it comprises Friedel-Crafts acylation reaction, chlorination, ring Oxidation, morpholino substitution, methylthio substitution, and refining steps; 30% liquid caustic soda is added as a catalyst in the morpholine substitution reaction. In addition to the risk of strong corrosion during operation, more importantly, it is in contact with epoxy During the nucleophilic reaction process of the intermediate, there are a large number of hydroxide anions in the high-concentration liquid caustic soda, and there is a strong competitive relationship with the substitution reaction of morphine. At the same time, the strong alkalinity of the reaction system also increases the possibility of elimination reaction. The elimination product will further react with morphine, resulting in poor product purity and difficult purification

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