- Method for visible light driven green synthesis of benzoin bis-ether
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The invention relates to a method for visible light driven green synthesis of benzoin bis-ether. The method comprises the steps that an alkyne compound, an alcohol compound and 10-methyl-9-sym-trimethylbenzene based acridine perchlorate perform driving reaction in the atmosphere at room temperature with the visible light with the wavelength of 450-460 nm, a reaction solution is obtained after 3 hours and is spin-dried to obtain concentrate, and the concentrate is subjected to column chromatography on silica gel to obtain the benzoin bis-ether. The method is high in yield, moderate in conditionand small in environmental pollution.
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Paragraph 0022-0029
(2019/02/10)
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- Visible-light-enabled aerobic synthesis of benzoin bis-ethers from alkynes and alcohols
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A new, facile, atom-economical and good regioselective method for the synthesis of benzoin bis-ethers has been developed via directly using readily available alkynes and alcohols as raw materials under visible light irradiation. The protocol utilizes commercial Mes-Acr+ClO4- as an organophotoredox catalyst and air (O2) as a green sustainable reagent. A range of benzoin bis-ether derivatives were easily and efficiently obtained in a one-pot procedure at room temperature, and water is the by-product.
- Lei, Wen-Long,Yang, Biao,Zhang, Qing-Bao,Yuan, Pan-Feng,Wu, Li-Zhu,Liu, Qiang
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supporting information
p. 5479 - 5483
(2019/01/03)
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- A benzion double-methyl ether synthesis process
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The present invention discloses a benzoin dimethyl ether synthesis process, which comprises: adding methanol, benzaldehyde, sodium cyanide and water to a reaction kettle, carrying out a condensation reaction to generate an intermediate benzoin, adding the benzoin to an oxidation kettle, carrying out an oxidation reaction to obtain dibenzoyl, adding the dibenzoyl to a synthesis kettle, adding dimethyl sulfate and solvents such as dioxane and sodium methoxide, carrying out alkali fusion, adding water after the alkali fusion, carrying out thermal insulation at a temperature of 70 DEG C, carrying out alkali crystal layering, adding water to the crystal layer, carrying out cooling crystal transition, placing into a centrifuge to dewater, carrying out water washing centrifugation to obtain a crude wet product, pouring the crude wet product into a refining kettle, adding methanol through a metering pump, heating to a temperature of 60 DEG C to dissolve, adding active carbon, carrying out decolorization, filtering after the decolorization so as to remove the active carbon, conveying the filtrate into an crystallization kettle, carrying out cooling crystallization for 3 h to obtain a wet fine product, drying the wet fine product through filtration, washing and drying three-in-one equipment to obtain the finished product, and carrying out packaging warehousing. With the synthesis process of the present invention, the effects of low raw material cost, low environmental pollution, and high finished product yield are achieved.
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Paragraph 0039; 0040; 0041; 0042; 0043; 0044; 0045
(2017/04/29)
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- Oxidation of alcohols and activated alkanes with lewis acid-activated tempo
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The reactivity of MCl3(η1O) (M = Fe, 1; Al, 2; TEMPO = 2,2,6,6-tetramethylpiperidine-N-oxyl) with a variety of alcohols, including 3,4-dimethoxybenzyl alcohol, 1-phenyl-2-phenoxyethanol, and 1,2-diphenyl-2-methoxyethanol, was investigated using NMR spectroscopy and mass spectrometry. Complex 1 was effective in cleanly converting these substrates to the corresponding aldehyde or ketone. Complex 2 was also able to oxidize these substrates; however, in a few instances the products of overoxidation were also observed. Oxidation of activated alkanes, such as xanthene, by 1 or 2 suggests that the reactions proceed via an initial 1-electron concerted proton-electron transfer (CPET) event. Finally, reaction of TEMPO with FeBr3 in Et2O results in the formation of a mixture of FeBr3(η1OH) (23) and [FeBr2(η1OH)]2(μ-O) (24), via oxidation of the solvent, Et2O.
- Nguyen, Thuy-Ai D.,Wright, Ashley M.,Page, Joshua S.,Wu, Guang,Hayton, Trevor W.
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p. 11377 - 11387
(2015/02/19)
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- COLORED CURABLE COMPOSITION, FLUORINE-CONTAINING DIPYRROMETHENE COMPOUND AND TAUTOMER THEREOF, AND FLUORINE-CONTAINING DIPYRROMETHENE METAL COMPLEX AND TAUTOMER THEREOF, AND COLOR FILTER USING THE SAME AND METHOD FOR PRODUCING THE COLOR FILTER
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A colored curable composition contains a dipyrromethene metal complex compound formed from a fluorine-containing dipyrromethene compound represented by Formula (1) and a metal or metal compound. (R1 to R7: H or substituent (at least one of R1 to R7 includes a substituent represented by Formula (2)); Rg: H or substituent; a ≧1; Rf: a fluorine atom, fluorine-containing alkyl group having 1 to 4 carbon atoms, fluorine-containing aryl group, fluorine-containing alkoxy group having 1 to 4 carbon atoms, fluorine-containing alkylsulfonamido group having 1 to 4 carbon atoms, or fluorine-containing arylsulfonamido group; m: 1 to 5; n: 0 to 4; L: single bond, O, S, NH, R—NH(R: alkylene), —Ar—NH— (Ar: arylene), CO, COO, OCO, *COS, *SCO, *CONH, *NHCO, *NHSO2, SO, SO2, *SO2NH, an alkylene chain having 1 to 4 carbon atoms or arylene group.)
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- COLORED CURABLE COMPOSITIONS, COLOR FILTERS AND PROCESS FOR PRODUCTION THEREOF
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The present invention provides a compound represented by the following Formula (C1), or a colored curable composition containing a tetraazaporphyrin colorant having at least one group represented by the following Formula (I), and a color filter using the composition and a manufacturing method thereof: wherein Rc1: a halogen atom, aliphatic group, aryl group, heterocyclic group, cyano group, carboxyl group, carbamoyl group, aliphatic oxycarbonyl group, aryloxycarbonyl group, acyl group, hydroxyl group, aliphatic oxy group, aryloxy group, etc.; Zc1: a non-metal atom group necessary for forming a 6-membered ring together with the carbon atom; M: two hydrogen atoms, a divalent metal atom, divalent metal oxide, divalent metal hydroxide, divalent metal chloride; cm= 0 to 2, cn= 0, 1 to 5; cr1, cr2, cr3, cr4= 0 to 1 (cr1 + cr2 + cr3 + cr4 ≥ 1); L1: an alkylene group; A1 and A2: -O-, -C(=O)-, -OC(=O)-, -C(=O)O-, -N(R2)C(=O)-, -C(=O)N(R2)-, -N(R2)C(=O)-, -OC(=O)N(R2)-, N(R2)C(=O)N(R3)-, -N(R2)SO2-, -SO2N(R2)-, or -SO2-; L2: an alkylene group, aralkylene group, or arylene group; n: an integer from 1 to 3; m: an integer from 0 to 3; R1: a hydrogen atom, alkyl group, aryl group or heterocyclic group; and R2 and R3: a hydrogen atom, alkyl group, aryl group or heterocyclic group.
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- Anodic oxidation of benzil hydrazones in the presence of halide ions
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Benzil hydrazones were subjected to electrolytic oxidation in MeOH containing halide ion source, such as KI and KBr. The results show that the reaction products were dependent on both the electrolytes and the substituents. In the presence of KI, benzoylphenyldiazomethanes were obtained, whereas in the presence of KBr, benzil dimethyl acetals were obtained.
- Okimoto, Mitsuhiro,Takahashi, Yukio
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p. 2059 - 2060
(2007/10/03)
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- Dioxirane formation in ozonolysis of E- and Z-1,2-dimethoxy-1,2-diphenylethene
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Addition of ozone to E- and Z-1,2-dimethoxy-1,2-diphenylethene, E- or Z-1, in inert solvents results in formation of ca 1 mole of methyl benzoate, ca 0.5 and ca 0.1 mole of the corresponding oxiranes 2 and dioxetanes 3, respectively, and 0.03 mole of 3,6-dimethoxy-3,6-diphenyl-1,2,4,5-tetroxane 4 at -20 deg C.Product distributions vary with starting material, initial concentration, extent of reaction, and temperature.At -70 deg C ca 0.3 mole of trans-2 and 0.2 mole of cis- and trans-4 are formed from E-1.Addition of E- or Z-1 to solutions of excess ozone results in formation of up to 0.7 mole of (methoxy)phenyldioxirane 5, which is a strong, stereospecific epoxidizing agent.
- Kopecky, Karl R.,Xie, Yu,Molina, Jose
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p. 272 - 274
(2007/10/02)
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- Selenium-Mediated Conversion of Alkynes into α-Dicarbonyl Compounds
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The reaction of terminal and internal alkynes with diphenyl diselenide and ammonium peroxydisulfate in methanol proceeds smoothly to give α-keto acetals and α-keto ketals, respectively.This one-pot procedure is suggested to proceed through the initial formation of phenylselenenyl sulfate, a strong electrophilic reagent which effects the methoxyselenenylation of the alkynes.The addition products thus formed suffer methoxydeselenenylation giving the observed products and regenerating the phenylselenenylating agent.In some cases the reaction can be carried out using only catalytic amounts of diphenyl diselenide.The same reaction carried out in the presence of water or of ethylene glycol gives the unprotected or the diprotected α-dicarbonyl compounds, respectively.
- Tiecco, Marcello,Testaferri, Lorenzo,Tingoli, Marco,Chianelli, Donatella,Bartoli, Donatella
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p. 4529 - 4534
(2007/10/02)
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- Preparation of symmetric and asymmetric monoacetals of aromatic 1,2-diketones
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Symmetric and asymmetric monoacetals of aromatic 1,2-diketones are prepared by a novel process, in a nonpolar solvent in the presence of a urea derivative as the catalyst.
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- Dental composite and porcelain repair
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A filled-resin composition useful for porcelain repair and as a dental composite and therefore made up of non-toxic materials and a method for repairing porcelain or teeth. The composition comprises a methacrylate functional resin usable in dental composites, powdered filler-colorant therein, at least one photoinitiator for the resin in an amount sufficient to initiate polymerization and complete it in depth within about half a minute when exposed to a visible-light output of at least 5,000 foot candles, the photoinitiator being an exciplex of (1) an carbocyclic ketone or acetal and (2) either ethyl-4-dimethyl amino benzoate or ethyl-2-dimethyl amino benzoate, and at least one accelerator-free peroxide curing agent for the resin in an effective amount for completing polymerization within about one-half hour of any portion of the resin not receiving sufficient light to effectuate complete cure before then. The method comprises mixing the components together under ordinary indoor lighting conditions, emplacing the mixture within a few minutes of the mixing, and curing at least a substantial portion of the emplaced mixture in situ for one half-minute under intense visual-light illumintion of at least 5000 foot-candles. Any resin then uncured by light is cured within the next half hour by the peroxide curing agent.
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- Conductive adhesive and biomedical electrode
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A biomedical electrode having a conductive adhesive thereon which is derived from an essentially solventless process. The resulting adhesive is characterized in that it is a swellable, dermally-nonirritating conformable, coadhesive, ionic, hydrophilic polymer.
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- Manufacture of symmetrical or unsymmetrical monoacetals of aromatic 1,2-diketones
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Monoacetals of aromatic 1,2-diketones are manufactured by reacting the corresponding 1,2-diketones, in an organic solvent, with an acid ester (R1)n X as alkylating agent and an alcoholate (R2 O)m Me, where R1 and R2 are identical or different hydrocarbon radicals of 1 to 12 carbon atoms, which may or may not be substituted, n and m are integers from 1 to 3, X is a monobasic, dibasic or tribasic acid radical and Me is a metal of main groups 1 to 3 of the periodic table of the elements. The resulting diketone monoacetals are particularly suitable for use as photoinitiators in photopolymerizable compositions.
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- Monoacetals or aromatic 1,2-diketones
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Monoacetals of aromatic diketones in which the acetal group is derived from primary mono- or dialkohols are useful as sensitizers in the photochemical polymerization or photochemical crosslinking of polymers. They are prepared from the diketones (benzils) by reaction with sulfites. The sulfites and the benzils may be formed immediately before the reaction in the same vessel without isolating these compounds. Most of the benzil monoacetals are new compounds.
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- Oxidation of Diphenylacetylene by I7+ and I5+ Compounds
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The oxidation of diphenylacetylene with H5IO6 in acetic acid affords benzil.In methanol the principal products are the monoketal and the diketal of benzil, depending upon water content.Similar products are formed in methanol when I2O5 is the oxidizing agent.The latter and the alkyne in ethylene glycol afford benzil and the corresponding diketal.Both systems appear to require the presence of iodine for effective action.
- Gebeyehu, Gulilat,McNelis, Edward
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p. 4280 - 4283
(2007/10/02)
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