947-19-3Relevant academic research and scientific papers
O-hydroxyketoxime compound as well as preparation method and application thereof
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Paragraph 0088-0091, (2022/03/18)
The invention relates to an o-hydroxyketoxime compound as well as a preparation method and application thereof. The o-hydroxyketoxime compound has a structural formula as shown in a formula (I) or a formula (II) which is described in the specification. The o-hydroxyoxime compound provided by the invention has adjacent hydroxyl group and oxime group structures, forms a specific hydrophobic structure with R1, R2 and R3 groups, has better chelating ability to metal ions, has particularly excellent chelating ability to Cu (II), and is excellent in flotation effect; and compared with salicylaldoxime, the recovery rate of the compound of the invention is increased by 1-30%, and the compound can be widely applied to flotation of copper oxide.
Preparation method of photoinitiator
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Paragraph 0074-0105, (2021/10/13)
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.
Oxidation of Primary Alcohols and Aldehydes to Carboxylic Acids via Hydrogen Atom Transfer
Tan, Wen-Yun,Lu, Yi,Zhao, Jing-Feng,Chen, Wen,Zhang, Hongbin
supporting information, p. 6648 - 6653 (2021/09/08)
The oxidation of primary alcohols and aldehydes to the corresponding carboxylic acids is a fundamental reaction in organic synthesis. In this paper, we report a new chemoselective process for the oxidation of primary alcohols and aldehydes. This metal-free reaction features a new oxidant, an easy to handle procedure, high isolated yields, and good to excellent functional group tolerance even in the presence of vulnerable secondary alcohols and tert-butanesulfinamides.
Synthesis method of photoinitiator 1-hydroxycyclohexyl phenyl ketone
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Paragraph 0023-0028, (2020/12/05)
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.
Method for preparing alpha-hydroxy ketone photoinitiator in microreactor
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Paragraph 0024; 0025; 0030; 0031, (2020/05/05)
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.
Directed Hydroxylation of sp2 and sp3 C-H Bonds Using Stoichiometric Amounts of Cu and H2O2
Trammell, Rachel,D'Amore, Lorenzo,Cordova, Alexandra,Polunin, Pavel,Xie, Nan,Siegler, Maxime A.,Belanzoni, Paola,Swart, Marcel,Garcia-Bosch, Isaac
supporting information, p. 7584 - 7592 (2019/06/11)
The use of copper for C-H bond functionalization, compared to other metals, is relatively unexplored. Herein, we report a synthetic protocol for the regioselective hydroxylation of sp2 and sp3 C-H bonds using a directing group, stoichiometric amounts of Cu and H2O2. A wide array of aromatic ketones and aldehydes are oxidized in the carbonyl γ-position with remarkable yields. We also expanded this methodology to hydroxylate the β-position of alkylic ketones. Spectroscopic characterization, kinetics, and density functional theory calculations point toward the involvement of a mononuclear LCuII(OOH) species, which oxidizes the aromatic sp2 C-H bonds via a concerted heterolytic O-O bond cleavage with concomitant electrophilic attack on the arene system.
Ultrasonic preparation method for alpha-hydroxyketones
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Paragraph 0032-0035, (2019/05/11)
The invention relates to the technical field of organic synthesis, and concretely relates to an ultrasonic preparation method for alpha-hydroxyketones. Ketones and peroxide which are used as raw materials undergo an ultrasonic reaction in the presence of an organic solvent to prepare the alpha-hydroxyketones. The preparation method provided by the invention avoids the use of halogens with high toxicity and high risks in the reaction process to avoid the risk of the product not meeting the requirements of the regulations due to the introduction of the halogens in the reaction process, and alsohas the advantages of low cost of the overall process, shortening of the cycle of batch production, simplicity in process operation and easiness in achieving of large-scale production.
Photocatalytic synthesis method of 1-hydroxyl cyclohexyl phenyl ketone compound and application thereof
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Paragraph 0019; 0020, (2019/03/08)
A photocatalytic synthesis method of a 1-hydroxyl cyclohexyl phenyl ketone compound comprises the following steps that (a) 4-Ryl benzaldehyde and cyclohexane produce free radical reaction under the irradiation of an ultraviolet lamp to obtain 4-Ryl cyclohexyl phenyl ketone; (b) the 4-Ryl cyclohexyl phenyl ketone uses dimethyl sulfoxide as a solvent, uses hydrobromic acid as a bromine source, hydroxyl substitution is performed to obtain 1-hydroxyl cyclohexyl-(4-R phenyl) ketone, and the dimethyl sulfoxide is removed for recycle through distillation. A 1-hydroxyl cyclohexyl-(4-R phenyl) ketone coarse product is obtained through a crystallization method, and a 1-hydroxyl cyclohexyl-(4-R phenyl) ketone photoinitiator finished product is obtained through recrystallization. The synthesis methodhas the advantages that the synthesis steps of the method are simple, the preparation cost is low and no pollution is produced. The prepared cyclohexyl phenyl ketone compound is suitable for the efficient photoinitiator of UV light curing system, the product has better non-yellowing characteristic under the irradiation of an ultraviolet source, and popularization and development of a UV light curing technology are facilitated.
Expedient preparation of active pharmaceutical ingredient ketamine under sustainable continuous flow conditions
Kassin, Victor-Emmanuel H.,Gérardy, Romaric,Toupy, Thomas,Collin, DIégo,Salvadeo, Elena,Toussaint, Fran?ois,Van Hecke, Kristof,Monbaliu, Jean-Christophe M.
supporting information, p. 2952 - 2966 (2019/06/18)
A robust three-step continuous flow procedure is presented for the efficient and sustainable preparation of active pharmaceutical ingredient ketamine. The procedure relies on the main assets of continuous flow processing, starts from commercially available chemicals, utilizes low toxicity reagents and a FDA class 3 solvent under intensified conditions. The procedure features a unique hydroxylation step with molecular oxygen, a fast imination relying on triisopropyl borate and a thermolysis employing Montmorillonite K10 as a heterogeneous catalyst, all three steps being performed in ethanol. The three individual steps can be run independently or can be concatenated, thus providing a compact yet efficient setup for the production of ketamine. The scalability of the critical hydroxylation step was assessed in a commercial pilot continuous flow reactor. The process can also be adapted for the preparation of ketamine analogs. A thorough computational study on the backbone rearrangement of the cyclopentylphenylketone scaffold under thermal stress rationalizes the experimental selectivity and the various experimental observations reported herein.
Preparation method of photoinitiator 184
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Paragraph 0033-0034, (2019/04/04)
The invention relates to a preparation method of a photoinitiator 184, in particular to the preparation of the photoinitiator 184 from 1-halocyclohexyl phenyl ketone through a hydrolysis reaction in the presence of quaternary ammonium base. By the preparation method, provided by the invention, the reaction is clean, recrystallization purification can be directly performed, and a qualified productcan be prepared; the occurrence of side reactions is avoided or reduced, the yield is increased, and the preparation method is suitable for industrial production in terms of cost and operation.
