- Method for efficiently rectifying and producing tetraethyl orthocarbonate
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The invention relates to the field of refining chemicals and specifically relates to a method for efficiently rectifying and producing tetraethyl orthocarbonate. According to the method, a low-polarity inert solvent is used for treating tetraethyl orthocarbonate, so that the extracting function is achieved, less water can be co-boiled and brought away in a rectifying process and the product is prevented from degrading in the rectifying process; the solid alkali is added, so that the pH value of the rectifying system is increased and the product is prevented from continuously degrading under the effect of pH value decreasing in the rectifying process; the technical measure is adopted for acquiring the efficiently rectified and stably produced high-purity tetraethyl orthocarbonate. Comparedwith the present technology, the method provided by the invention has the characteristics of high efficiency, stability, and the like, the high-purity product can be continuously rectified and separated and the purity of the product can reach up to 99.5% or above.
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Paragraph 0023-0028; 0029-0034; 0035-0040; 0041-0046
(2018/04/02)
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- A method for synthesizing original ester carbonate (by machine translation)
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The invention relates to a synthesis method of carbonic acid ortho-ester. The synthesis method of the carbonic acid ortho-ester comprises the following steps: (1) preparing crude carbonic acid ortho-ester from tetrahalomethane under the action of alcohol and an alkali metal hydroxide or an alkali metal compound of alcohol, wherein a synthesis reaction equation of the carbonic acid ortho-ester is described in the specification; (2) filtering and removing halide, so that a carbonic acid ortho-ester-alcohol solution is obtained; and (3) carrying out reduced pressure rectification, so that refined carbonic acid ortho-ester is obtained. The synthesis method of the carbonic acid ortho-ester has the advantages that the operation is simple, virulent raw materials and auxiliary materials or auxiliary materials capable of producing highly toxic substances in the traditional technology are abandoned, the emission of three wastes and the cost are greatly reduced, environmental friendliness is realized, and the synthesis method of the carbonic acid ortho-ester is applicable to large-scale production.
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Paragraph 0023; 0024
(2020/02/07)
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- Mechanistic study of the ring-size modulation in Michael-Dieckmann type reactions of 2-acylaminoacrylates with ketene diethyl acetal
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An unexpected modulation of the chemoselectivity in the Michael-Dieckmann type reactions of 2-acylaminoacrylates with ketene diethyl acetal is observed, depending on the nature of the acylamino group. Experimental and theoretical studies are presented to offer insights into the origin of this substituent effect in terms of a polar stepwise mechanism. The Royal Society of Chemistry and the Centre National de la Recherche Scientifique.
- Avenoza, Alberto,Busto, Jesus H.,Canal, Noelia,Garcia, Jose I.,Jimenez-Oses, Gonzalo,Peregrina, Jesus M.,Perez-Fernandez, Marta
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p. 224 - 229
(2008/02/02)
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- CRYSTAL AND PROCESS FOR PRODUCING THE SAME
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A process for producing crystals of 2-ethoxy-1-[[2'-(1H-tetrazol-5-yl)biphenyl-4-yl]methyl]-1H-benzimdazole-7-carboxylic acid (compound (I)), characterized by dissolving or suspending the compound (I) or a salt thereof in a solvent comprising an aprotic polar solvent and crystallizing it. By the process, the contaminants which are contained in the compound (I) or its salt and are difficult to remove, such as tin compounds, analogues of the compound (I), and a residual organic solvent, can be easily removed. Crystals of the compound (I) can be efficiently and easily mass-produced in high yield on an industrial scale.
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- Process for the preparation of orthocarbonates
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Orthocarbonates are prepared by a process, comprising: reacting trichloroacetonitrile with an alkali metal salt or alkaline earth metal salt of an alcohol of the formula: R—OH??(II) wherein R is an unsubstituted or substituted, saturated aliphatic or cycloaliphatic hydrocarbon radical in which the carbon atom of group R, linked to the oxygen atom of the alcohol, has at least one hydrogen atom, reacting the product obtained in water with an oxidant, extracting the organic-aqueous phase of the material obtained after oxidation, and distilling the extracted material obtained and obtaining orthocarbonate product of the formula: C(OR)4??(I) wherein each R group is as defined above.
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Page column 4-5
(2008/06/13)
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- Photopolymerizable vinyl ether based monomeric formulations and polymerizable compositions which may include certain novel spiroorthocarbonates
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Photopolymerizable compositions are provided which are the reaction products of a vinyl ether, a photoinitiator system comprising an iodonium salt, a visible light sensitizer, and an electron donor compound. These monomeric/oligomeric compositions may also include epoxides, polyols, spiroorthocarbonates. One embodiment of the present invention is a polymerizable composition comprised of a vinyl ether, a spiroorthocarbonate, and a photoinitiator system. Another embodiment of the present invention is a polymerizable composition comprised of a vinyl ether, an epoxide, a polyol, and a photoinitiator system. Still another embodiment of the present invention is a polymerizable composition comprised of a vinyl ether, an epoxide, a polyol, a spiroorthocarbonate, and a photoinitiator system. Still further, another embodiment of the present invention is certain novel spiroorthocarbonate compounds. Each of these novel spiroorthocarbonate compounds include at least one epoxy group as a substituent.
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- Silver(I) ion-mediated desulfurization-condensation of carbon disulfide with some hydroxyl compounds
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The title reaction with ethanol and phenol gave tetraethyl and tetraphenyl orthocarbonate, respectively, in good yields. Diols, such as benzene-1,2-dimethanol, wieso-hydrobenzoin, and cathecol, afforded spiro orthocarbonic acid esters. In the same manner, 2-anilinoethanol, N-methylanthranilic acid, and salicylic acid led to some novel spirobicycles.
- Shibuya, Isao,Gama, Yasuo,Shimizu, Masao
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p. 461 - 464
(2007/10/03)
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- Ein neuer Zugang zu Spiroorthocarbonaten und neuen Orthokohlensaeure-Derivaten
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New and simple processes have been developed, which give in good or excellent yields new diphenoxyalkanediyldioxymethanes, symmetrical and unsymmetrical spiroorthocarbonates, spirocyclic orthothiocarbamic acid esters, and acetals of urea by successive or simultaneous substitution of chloro and phenoxy groups contained in dichlorodiphenoxymethane.
- Mues, Peter,Buysch, Hans-Josef
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p. 249 - 252
(2007/10/02)
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- Orthoamides, XXXVIII. - Contributions to the Chemistry of Orthocarbonic Acid Esters and α,α,α-Trialkoxyacetonitriles
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The reactivity of the orthocarbonates 4 and the nitriles 1 has been investigated.Carboxylic acids are esterified by 4b. Orthocarbonates 4c-f and 9b are prepared by transesterification of 4b.Mixed substituted orthocarbonates 8c-f are obtained from the nitriles 1a,b.The nitriles 2a and 3a react with alkali alcoholate in alcohol to yield the orthocarbamic acid esters 13a,b. Spirocyclic orthocarbonates 17a-d are prepared from 4b and 1,2 or 1,3-dioles, respectively. The reaction of phenol with 1b affords the mixed substituted orthocarbonate 18a. Catechol is converted by 1a into the orthocarbonate 20a.Reactions of 4b with amines and ami ne derivatives are studied. In the course of these investigations guanidines 21, imidocarbonic acid esters 22a-c, 30, carbamic acid esters 25, ureas 26, the isourea derivative 29, as well as the 1,3,4-oxadiazole 31 are prepared. The mechanism of these reactions is discussed. Imidocarbonic acid esters 22d-f, 38, N-cyanocarbamates 39, and isoureas 37 can be prepared from 1b and amines or amine derivatives. 2a as well as 13b react with cyanamide to give the N-cyanoisourea 40. Ureas 26 are formed in the reaction of 1a,b with secondary amines at elevated temperatures.The guanidinium cyanide 41a can be obtained by reaction of pyrrolidine with 1b in ether, whereas under similiar conditions from 1a and pyrrolidine the amidine 42 is produced. o-Aminophenol, o-phenylenediamine and anthranilic acid are cyclized by 4b or 1b to afford the heterocyclic compounds 43-45. α- and β-amino acids are transformed by 4b or 1b into the N-(ethoxycarbonyl)amino acid esters 46 and 47, respectively.
- Kantlehner, Willi,Maier, Thomas,Loeffler, Wolfgang,Kapassakalidis, Joanis J.
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p. 507 - 529
(2007/10/02)
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- Orthoamides, XXXV. - Preparation of O,N-Functional Trisubstituted Acetonitriles
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Trichloroacetonitrile (7) reacts with molar amounts of alcoholates in alcohols to give mixtures of orthocarbonates 10 and trichloroacetimidates 9.The action of 7 on 3 moles of sodium ethoxide in heptane affords triethoxyacetonitrile 3b among other products, such as 9b, 10b and the imidate 12.The nitrile 3a can be obtained from 7 and sodium methoxide in ether in moderate yields. - The orthocarbonic acid derivatives 10b, 20a and 21a are transformed by acyl cyanides into the nitriles 3b, 4a, and 5a, respectively.N,N,N',N',N'',N''-hexamethylguanidinium cyanide (23a) is f ormed in the reaction of 22 with acetyl cyanide. - The salts 30a-32a react with alkali cyanides to form the nitriles 3b, 4a, and 5a, respectively.The nitrile 2a transfers cyanide ions to the carbenium ions 30a and 31a to yield the nitriles 3b and 4a, respectively.
- Kantlehner, Willi,Maier, Thomas,Kapassakalidis, Joannis J.
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