- 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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Paragraph 0034-0073
(2021/10/13)
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- Preparing method of photoinitiator 2-methyl-2-hydroxy-1-phenylacetone
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The invention discloses a preparing method of a photoinitiator 2-methyl-2-hydroxy-1-phenylacetone. The preparing method comprises the steps of conducting acylation reaction on isobutyric acid and phosphorus trichloride, after the reaction is completed, introducing hydrogen chloride gas to make the intermediate state reaction complete, obtaining 2-chloride-2-methyl propionylchloride through chlorination reaction, conducting Friedel-Crafts reaction with benzene in the presence of a catalyst to obtain 2-chloride-2-methyl-1-phenylpropane-1-ketone, and finally after alkaline hydrolysis, washing anddistillation, obtaining the photoinitiator 1173. According to the preparing method, hydrogen chloride is introduced into the acylation step, so that the reaction yield is increased, and byproduct odors are reduced; meanwhile, chlorination reaction of a conventional technology is conducted one step in advance, the production cost of the conventional technology is reduced, and thus the product hasmarket competitiveness.
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Page/Page column 4-6
(2019/04/30)
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- New synthesis technology for photoinitiator1173
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The invention relates to a midbody isobutyrophenone of a photoinitiator1173 (2-hydroxy-2-methyl-1-phenyl-1-acetone) and a new synthesis technology for a photoinitiator1173. The new synthesis technology includes the steps that isobutylbenzene serves as a raw material, an oxidizing reaction is carried out with oxygen under the catalytic effect of catalyst cobalt salt or palladium salt, and the isobutyrophenone is obtained; the isobutyrophenone is further chloridized and hydrolyzed with a sodium hydroxide solution, and the photoinitiator1173 is obtained. The influence of the catalyst cobalt salt or palladium salt on isobutyrophenone production in the reaction is inspected, the material ratio in the isobutyrophenone and photoinitiator1173 production is determined, and the new technology is easy to operate and economical.
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- Dichloromethane as a chlorination reagent for α-bromocarbonyl compounds in the presence of a copper catalyst
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We found that dichloromethane is a powerful chlorinating reagent for the congested 3° and 2° Csp3Br bond of α-bromocarbonyl amides, esters, and ketones. In the presence of an appropriate copper complex as a catalyst, the desired chlorination occurred within an hour. Control experiments revealed that in situ-generated CuCl2 is a key chlorinating agent that reacts with the 3° or 2° alkyl radicals generated by the reaction between an α-bromocarbonyl compound and a Cu(I) salt.
- Takeuchi, Kentaro,Ishida, Syo,Nishikata, Takashi
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supporting information
p. 644 - 646
(2017/08/30)
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- 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone synthesis process
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The present invention discloses a 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone synthesis process, which is characterized in that isobutyric acid is adopted as a raw material, an acylation reaction, a Friedel-Crafts reaction, and an alkaline hydrolysis reaction are performed to obtain a 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone crude product, and fine steaming is performed to obtain the 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone finished product. According to the present invention, the process is reasonable, no sulfur dioxide gas emits during the production process, the environmental pollution caused by the produced sodium chloride is low, and the product yield is high.
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Paragraph 0010
(2017/06/21)
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- Iodine(III)-Mediated Oxidative Hydrolysis of Haloalkenes: Access to α-Halo Ketones by a Release-and-Catch Mechanism
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An unprecedented iodine(III)-mediated oxidative transposition of vinyl halides has been accomplished. The products obtained, α-halo ketones, are useful and polyvalent synthetic precursors. There are only a handful of reported examples of the direct conversion of vinyl halides to their corresponding α-halo carbonyl compounds. Insights into the mechanism and demonstration that this synthetic transformation can be done under enantioselective conditions are reported.
- Jobin-Des Lauriers, Antoine,Legault, Claude Y.
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supporting information
p. 108 - 111
(2016/01/15)
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- Silver-catalyzed decarboxylative chlorination of aliphatic carboxylic acids
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Decarboxylative halogenation of carboxylic acids, the Hunsdiecker reaction, is one of the fundamental functional group transformations in organic chemistry. As the initial method requires the preparations of strictly anhydrous silver carboxylates, several modifications have been developed to simplify the procedures. However, these methods suffer from the use of highly toxic reagents, harsh reaction conditions, or limited scope of application. In addition, none is catalytic for aliphatic carboxylic acids. In this Article, we report the first catalytic Hunsdiecker reaction of aliphatic carboxylic acids. Thus, with the catalysis of Ag(Phen)2OTf, the reactions of carboxylic acids with t-butyl hypochlorite afforded the corresponding chlorodecarboxylation products in high yields under mild conditions. This method is not only efficient and general, but also chemoselective. Moreover, it exhibits remarkable functional group compatibility, making it of more practical value in organic synthesis. The mechanism of single electron transfer followed by chlorine atom transfer is proposed for the catalytic chlorodecarboxylation.
- Wang, Zhentao,Zhu, Lin,Yin, Feng,Su, Zhongquan,Li, Zhaodong,Li, Chaozhong
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experimental part
p. 4258 - 4263
(2012/04/10)
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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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Page/Page column 4
(2011/04/18)
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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 11
(2010/01/29)
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- Process for preparing 1-indanones
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The present invention relates to a process for preparing 1-indanones of formula I: and isomers thereof, wherein R1, R2, R3, R4, R5, and R6 independently represent H or a C1-C20 hydrocarbon group or R1 and R2 or R2 and R3 or R3 and R4 and/or R5 and R6 together with the carbon atoms to which they are attached form a saturated or unsaturated 5- or 6-membered ring, said hydrocarbon group and/or said ring optionally containing one or more hetero atoms, said ring optionally being substituted with a C1-C4 hydrocarbon group, said process comprising reacting a compound of formula II: wherein R1, R2, R3, R4, R5, and R6 have the same meaning as defined above, with a chlorinating agent, followed by reaction with a Friedel-Crafts catalyst. The invention further relates to the preparation of the corresponding indenes.
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- Sulfuranes with Oximate Axial Ligands
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New sulfuranes having one or two axial oximate (R2C=NO) ligands were synthesized.An improved sulfurane-forming step, involving a rapidly stirred suspension of NaHCO3, is described.The failure of sulfide oximes in which sulfur bears one or two tertiary carbons to form sulfuranes is explained by a C-S bond cleavage leading to tertiary carbocations.This represents a hitherto unanticipated limitation to the standard method of sulfurane synthesis.The X-ray crystal structure of one of the new sulfuranes, namely 2,2'-spirobi(4-phenyl-3H-1,2,5-oxathiazoline), is reported (R = 0.0368).An unusual feature was the quite compressed equatorial (C-S-C) angle, 102.6(1) deg.The S-O bond length, 1.846(2) Angstroem, was similar to S-O bond lenghths of sulfuranes having two axial carboxylate ligands.Since the oximate ligand has not been used previously in a 10-S-4 species, an assessment of its apicophilicity relative to other more common axial ligands was made by considering X-ray structural data, IR data, and ab initio calculations.These suggest that the R2C=NO ligand is as apicophilic as the hexafluorocumyloxy (ArC(CF3)2O) ligand.
- Hornbuckle, S. F.,Livant, P.,Webb, T. R.
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p. 4153 - 4159
(2007/10/02)
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- The chlorination of isobutyrophenone: determination of its pKa value and of the course of the reaction
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Chlorination of isobutyrophenone in alkaline aqueous solution leads to formation of α-hydroxyisobutyrophenone as the first detectable intermediate; a slow subsequent oxidation gives benzoate.From the rates of the initial chlorinations we have been able to determine the pKa value for the ketone as 18.18 +/- 0.50. α-Chloroisobutyrophenone undergoes surprisingly rapid alkaline hydrolysis, kOH = 71.9 +/- 1.5 M-1 s-1.
- Guthrie, J. Peter,Cossar, John
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p. 397 - 403
(2007/10/02)
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- Coupling of Enolates of Phenones with 2-Chloro-2-nitropropane
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Lithium enolates of acetophenone, α-methoxyacetophenone, propiophenone, meta- or para-substituted propiophenones, butyrophenone, isovalerophenone, 1-phenyl-1-hexanone, 1-indanone, 1-tetralone, or 1-benzosuberone react with 2-chloro-2-nitropropane in THF by free radical chain processes to produce ArCOCH(CMe2NO2)R or ArCOC(R)=CMe2 and when R H the product of oxidative dimerization, 2.The enolate anion of deoxybenzoin yields in a free radical chain process only the dimerization product.
- Russel, Glen A.,Mudryk, Boguslaw,Jawdosiuk, Mikolaj,Wrobel, Zbigniew
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p. 1879 - 1884
(2007/10/02)
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