- Preparation method of photoinitiator
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The invention discloses a preparation method of a photoinitiator. The preparation method comprises the following steps: acid chloride required for Fries reaction, aluminum trichloride and a solvent are mixed and then subjected to a Fourier reaction with benzene. Fries reaction intermediate purification method The Fourier reaction intermediate is mixed with chlorine for chlorination reaction, and the product of the chlorination reaction is subjected to gas-liquid separation to separate the gas. Reaction Section Step and The product purification step results in a photoinitiator finished product. To the technical scheme of the invention, the advantages of the traditional process of producing the photoinitiator are combined with the characteristics of the microchannel reactor to realize continuous preparation, the productivity can be improved, the production risk is reduced, the manpower and equipment investment are reduced, and the cost is further reduced.
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- Synthesis method of photoinitiator 1-hydroxycyclohexyl phenyl ketone
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The invention aims to solve the technical problems of an existing alpha-hydroxycyclohexyl phenyl ketone synthesis method, provides a synthesis method of a photoinitiator 1-hydroxycyclohexyl phenyl ketone, and belongs to the technical field of chemical synthesis. The synthesis method comprises the following steps: (1) reacting a halogenated benzene with magnesium particles to prepare a Grignard reagent, dropwise adding cyclohexylcarbonitrile into the prepared Grignard reagent, and after the reaction is completed, hydrolyzing to generate cyclohexyl phenyl ketone; and (2) reacting cyclohexyl phenyl ketone with chlorine to obtain 1-chlorocyclohexyl phenyl ketone, and carrying out a hydrolysis reaction on the 1-chlorocyclohexyl phenyl ketone and a sodium hydroxide aqueous solution under the action of a catalyst to obtain 1-hydroxycyclohexyl phenyl ketone. The method is simple in synthesis process, high in yield and suitable for industrial production.
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- Method for preparing alpha-hydroxy ketone photoinitiator in microreactor
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The invention relates to a method for preparing an alpha-hydroxy ketone photoinitiator in a microreactor. The method comprises the following steps: introducing chlorine into isobutyryl benzene servingas a raw material to obtain an intermediate chloroisobutyryl chloride, and carrying out alkaline hydrolysis on the intermediate under the action of an aqueous sodium hydroxide solution to obtain thealpha-hydroxy ketone photoinitiator. The preparation method of the alpha-hydroxy ketone photoinitiator has the advantages of high operation safety, high selectivity, small reaction volume, short reaction time, low equipment corrosion, low energy consumption and environment friendliness, and is a process method suitable for industrial production.
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Paragraph 0024; 0030
(2020/05/05)
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- Synthetic method of photoinitiator 1-hydroxycyclohexyl phenyl ketone
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The invention discloses a synthetic method of a photoinitiator 1-hydroxycyclohexyl phenyl ketone. The synthetic method comprises the following steps: enabling cyclohexanecarboxylic acid chloride and benzene to be subjected to electrophilic substitution reaction under the catalysis of Lewis acid to obtain cyclohexyl phenyl ketone; enabling the cyclohexyl phenyl ketone to react with hydrogen peroxide and a hydrochloric acid solution under the action of a molecular sieve catalyst to obtain 1-chlorocyclohexyl phenyl ketone; and enabling the 1-chlorocyclohexyl phenyl ketone and a sodium hydroxide aqueous solution to be subjected to hydrolysis reaction under the action of the catalyst to obtain the 1-hydroxycyclohexyl phenyl ketone. The synthetic method disclosed by the invention has the advantages that the raw materials are cheap, easily-available, safe and environmentally friendly; hydrogen chloride produced by electrophilic substitution reaction of acyl chloride under the catalysis of Lewis acid is fully utilized and recycled, thereby reducing the discharge of waste acid water and being friendly to the environment; and selective chlorination and hydrolysis are completed in the same reactor, the operation is simple, the loss is less, and the yield is high.
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- A austria peso star synthetic method
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The present invention discloses an orbifloxacin synthesis method, which comprises: adopting sparfloxacin as a raw material, carrying out a diazotization reaction under the effect of hydrochloric acid and sodium nitrite to obtain a diazonium salt solution, adding tetrafluoroboric acid to the diazonium salt solution in a dropwise manner, carrying out a fluorization reaction at a temperature of -10 DEG C, filtering the reaction solution after completing the reaction, taking the filter cake, washing with ethyl ether, drying, heating the dried product until no gas is generated to obtain an orbifloxacin crude product, and purifying the orbifloxacin crude product to obtain the orbifloxacin. According to the present invention, the sparfloxacin is utilized as the starting raw material and the diazotization reaction and the fluorization reaction are used to prepare the orbifloxacin, such that advantages of new process route, high product yield, low reaction cost and short reaction time are provided, and the method is the new economical and practical technology.
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Paragraph 0019; 0022; 0025-0030
(2017/08/10)
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- PROCESS FOR THE PREPARATION OF AROMATIC ALPHA-HYDROXY KETONES
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Process for the preparation of aromatic alpha-hydroxyketones (aromatic α-hydroxyketones) that does not require the use of chlorine, sulfuryl chloride or bromine and comprises the halogenation of an intermediate aromatic ketone with a hydrogen halide in the presence of an oxidising compound.
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- PROCESS FOR THE PREPARATION OF AROMATIC ALPHA-HYDROXY KETONES
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Process for the preparation of aromatic alpha-hydroxyketones (aromatic α- hydroxyketones) that does not require the use of chlorine, sulfuryl chloride or bromine and comprises the halogenation of an intermediate aromatic ketone with a hydrogen halide in the presence of an oxidising compound.
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Page/Page column 18
(2010/01/29)
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- 1,2-Addition of α,α,α-trichlorotoluene to ketones via a Mg Barbier reaction in DMF: New route to cycloalk-1-en-1-yl and alk-1-en-1-yl phenyl ketones
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The reductive cyclocondensation of α,α,α-trichlorotoluene to enolisable ketones enables the preparation of (cyclo)alken-1-en-1-yl phenyl ketones via the formation of an intermediate chlorooxirane. Copyright Taylor & Francis Group, LLC.
- Aaziz, Akima,Oudeyer, Sylvain,Leonel, Eric,Paugam, Jean Paul,Nedelec, Jean-Yves
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p. 1147 - 1154
(2008/02/01)
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- Synthesis and Structure-Activity Relationships of 5-Substituted 6,8-Difluoroquinolones, Including Sparfloxacin, a New Quinolone Antibacterial Agent with Improved Potency
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A series of 5,7-disubstituted 1-cyclopropyl-6,8-difluoro-4(1H)-oxoquinoline-3-carboxylic acids (10-36) were prepared; the C-5 substituent in these compounds comprised halo, hydroxy, mercapto, and amino groups and the C-7 functional group included variously substituted piperazines.In vitro antibacterial screening results indicated that the amino group was optimal among the C-5 substituents.A combination of the C-5 amino group and the C-7 3,5-dimethylpiperazinyl appendage in this series conferred the best overall antibacterial property with lack of adverse drug interactions.Compound 36k was superior to ciprofloxacin in both in vitro and in vivo potency and hence was selected as a promising candidate for an improved therapeutic agent.
- Miyamoto, Teruyuki,Matsumoto, Jun-ichi,Chiba, Katsumi,Egawa, Hiroshi,Shibamori, Koh-ichiro,et al.
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p. 1645 - 1656
(2007/10/02)
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- Improved process for the preparation of 5-amino-7-(substituted amino)-quinoline-3-carboxylic acids
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An improved process for the preparation of 5-amino--7-(substituted-amino)-quinoline-3-carboxylic acids, having known antibacterial activity, is described wherein a 5-fluoro-7-(protected and substituted-amino)-quinoline-3-carboxylic acid is converted to a 5-protected amino compound and where both protected amino groups are simultaneously removed to give the desired product.
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