- DESIGN, SYNTHESIS, AND PHOTOPHYSICAL PROPERTIES OF A NOVEL NIR II DYE FOR BIOLOGICAL IMAGING AND OPTOELECTRONIC DEVICES
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In one aspect, the disclosure relates to fluorescent dyes that absorb and emit in the near infrared II (NIR II) range of the electromagnetic spectrum, methods of making same, compositions comprising same and methods of using the compositions to perform imaging on biological samples, and optoelectronic devices using the dyes. The dyes are small organic molecules that are inexpensive and facile to produce, can be water-soluble, have tunable properties, and are biocompatible and/or possess low toxicity.
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- Novel process for preparing sodium tert-butoxide by using xylene as solvent
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The invention belongs to the technical field of manufacturing of fine chemical intermediates, particularly relates to a novel process for preparing sodium tert-butoxide by using dimethylbenzene as a solvent, and solves the technical problems that a traditional sodium tert-butoxide synthesis method in the prior art directly uses tert-butyl alcohol as a solvent, metal sodium is easy to oxidize, sodium sheets are easy to gather, the reaction contact area is reduced, the stirring load of a reaction kettle is indirectly increased, and the like. The novel process for preparing the sodium tert-butoxide by using the xylene as the solvent comprises the steps of preparation before reaction including reaction kettle cleaning, drying and gas replacement; adding materials for reaction, specifically, melting metal sodium in xylene, adding sodium hydride for dissolving under the protection of inert gas, and then adding tert-butyl alcohol for reaction; obtaining a product, specifically, removing sodium hydride after the reaction is finished, and recovering xylene; and obtaining the product sodium tert-butoxide. The preparation process is simple, the preparation condition is mild, the reaction safety is high, and the product purity is high.
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Paragraph 0027-0084
(2021/05/29)
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- Sodium tert-butoxide and preparation method thereof
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The invention discloses sodium tert-butoxide and a preparation method thereof. The preparation method comprises the following steps: (1) taking methylbenzene or heptanes as a reaction medium, adding sodium amide and tertiary butanol, mixing and stirring to dissolve to obtain a mixed solution; (2) heating the mixed solution to 70-110 DEG C for reaction to obtain a crude product of sodium tert-butoxide till the reaction is completed; (3) rectifying the crude product of the sodium tert-butoxide to obtain a finished product of the sodium tert-butoxide. The preparation method disclosed by the invention has relaxed reaction conditions, is small in danger in the production process, simple in aftertreatment process of products and short in drying time, and the product yield is up to 99% or above.
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Paragraph 0022; 0023; 0024; 0025; 0026; 0027
(2019/05/08)
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- Sodium tert-butoxide production technology
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Sodium tert-butoxide is a main chemical material. The brief production process comprises the following steps: adding metered 99% sodium amide into a reaction vessel, simultaneously slowly dropwise adding a certain amount of 99% anhydrous tert-butanol, stirring after dropwise adding, controlling temperature of the reaction vessel to 85 DEG C, carrying out thermal insulation and carrying out reflux reaction for 10 h; and carrying out distillation after the reaction, distilling off tert-butanol (reused in the reaction vessel) until there is no fraction, cooling to room temperature, discharging, and packaging to obtain a 98% sodium tert-butoxide finished product. The whole reaction yield is 76.3%. Three-stage condensation is adopted, including two-stage chilled brine condensation and first-stage water-cooling. Tert-butanol (boiling point is 82.8 DEG C) adopts three-stage condensation, condenser area is 20 m, and tert-butanol condensation efficiency is 98%.
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Paragraph 0002-0003
(2017/08/29)
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- Preparation method of di-tert-butyl dicarbonate
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The invention relates to a preparation method of di-tert-butyl dicarbonate and belongs to the technical field of synthesis of pharmaceutical intermediates. The preparation method comprises the following steps: adding metal sodium into xylol; heating to obtain sodium sand; then dropwise adding tert-butyl alcohol and carrying out pumping filtration to obtain sodium tert-butoxide; dissolving the sodium tert-butoxide into petroleum ether; introducing carbon dioxide and reacting to obtain a monoester sodium salt solution; adding a catalyst and slowly dropwise adding diphosgene to react; after reacting, standing and carrying out the pumping filtration; and washing with water, drying, distilling, cooling and crystallizing to obtain the di-tert-butyl dicarbonate. According to the preparation method, the sodium tert-butoxide is prepared from the metal sodium and the di-tert-butyl dicarbonate is prepared from the sodium tert-butoxide; a pumping filtration method is used for replacing a previous distillation method, so that the process is simpler and more energy is saved; the petroleum ether is used for replacing n-hexane and toluene, so that the production cost is reduced and a product is easier to purify; and finally, after the reaction, the pumping filtration is carried out and then water washing is carried out, so that the amount of wastewater is reduced and the environment-friendly treatment cost is reduced.
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Paragraph 0023
(2017/07/19)
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- Preparation method for low residual granular sodium alkoxide or potassium alcoholate
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The invention provides a preparation method for low residual granular sodium alkoxide or potassium alcoholate. The method includes using sodium or potassium and alcohol as raw materials, mixing the mixture with a solvent, reacting in inert gas atmosphere by using a microwave heating method, and removing the residual alcohol and solvent in the presence of microwave after the reaction to get the granular sodium alkoxide or potassium alcoholate. The microwave frequency is 2450 +/- 50 MHz. The method can prepare sodium alkoxide or potassium alcoholate with low residual solvent, and the prepared sodium alkoxide or potassium alcoholate is large granular solid, so that the development from powdered product to granular product can be realized, and the problems of residual solvent and potential risk troubled human for a long time can be overcome.
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Paragraph 0037-0038
(2017/01/17)
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- Amide acetals in the synthesis of pyridothienopyrimidines
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Methyl 3-amino-4-arylaminothieno[2,3-b]pyridine-2-carboxylates containing various substituents in the benzene ring were synthesized by the Thorpe-Ziegler reaction of 4-arylamino-2-chloropyridine-3-carbonitriles with methyl thioglycolates. The influence of the substituent in the benzene ring, acetal structure, the solvent and the process temperature on the reactions of obtained compounds with amide acetals was studied. It was established that reactions with dimethylacetamide dimethylacetal in toluene smoothly results in amidine derivatives, viz., methyl 4-arylamino-3-[1-(dimethylamino)ethylidene] aminothieno[2,3-b]pyridine-2-carboxylates, regardless of the substituent in the benzene ring. Analogous reaction of p-fluoroderivative with dimethylacetamide dimethylacetal in refluxing anhydrous ethanol leads to intramolecular cyclocondensation to produce substituted pyridothienopyrimidines, viz., 5H-1-thia-3,5,8-triazaacenaphthenes, in good yields. Amidine derivatives were the major products in the case of the coupling of aminothienopyridines with dimethylformamide dimethylacetal under the same conditions. A new approach to the synthesis of substituted pyridothienopyrimidines, viz., 3H-1-thia-3,5,8- triazaacenaphthylenes, based on the prolonged heating of methyl 4-arylamino-3-[1-(dimethylamino)ethylidene]aminothieno[2,3-b] pyridine-2-carboxylates in the excess of acetic anhydride was elaborated. Putative mechanisms of the processes concerned are given.
- Medvedeva,Tugusheva,Alekseeva,Chernyshev,Avramenko,Granik
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experimental part
p. 1946 - 1958
(2011/07/29)
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- 5-Oxo-5,8-dihydro-pyrido-pyrimidines as inhibitors of c-fms kinase
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The invention addresses the current need for selective and potent protein tyrosine kinase inhibitors by providing potent inhibitors of c-fms kinase. The invention is directed to the novel compounds of Formula I: or a solvate, hydrate, tautomer or pharmaceutically acceptable salt thereof, wherein:W, A, Y, n, Z, and R102 are described in the specification.
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Page/Page column 22; 34
(2008/06/13)
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- 5-Oxo-5,8-dihydro-pyrido-pyrimidines as inhibitors of c-fms kinase
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The invention addresses the current need for selective and potent protein tyrosine kinase inhibitors by providing potent inhibitors of c-fms kinase. The invention is directed to the novel compounds of Formula I: or a solvate, hydrate, tautomer or pharmaceutically acceptable salt thereof, wherein: W, A, Y, Z, R101 and R200 are described in the specification.
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Page/Page column 33; 39; 40; 66-67; 68
(2010/11/26)
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- Novel aminophenyl ketone derivatives
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Novel heteroaryl aminophenyl ketone derivatives which are inhibitors of MAP kinases, in particular the p38 MAP kinase, are useful as anti-inflammatory agents in the prophylaxis or treatment of inflammatory diseases or conditions.
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- Diamino isothiazole-1-oxides and 1,1 dioxides as gastric secretion inhibitors
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This invention is directed to diamino isothiazole -1-oxides and -1,1-dioxides and related compounds as well as pharmaceutical compositions and methods useful in the treatment of gastric secretion in mammals.
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- Process for producing azolylmethylcyclopentanol derivatives
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An azolylmethylcyclopentanol derivative which is useful as an agricultural and horticultural fungicide and which is represented by the formula (II) : wherein R1 represents a hydrogen atom or an alkyl group having 1 to 5 carbon atoms, R2 represents a hydrogen atom or an alkyl group having 1 or 2 carbon atoms, X represents a halogen atom, an alkyl group having 1 to 4 carbon atoms, a phenyl group, a cyano group, a trifluoromethyl group or a nitro group, A represents a nitrogen atom or a CH group and m is an integer of 1 to 5 is prepared by reacting a cyclopentanone derivative represented by the formula (I) : wherein R1, R2, X and m are as defined above, with an azole compound represented by the formula (III) : wherein A is as defined above and M represents an alkali metal atom or a hydrogen atom, and a sulfonium methylide or a sulfoxonium methylide in a polar solvent or a mixture of a polar solvent and an alcohol having 1 to 5 carbon atoms and, when M represents a hydrogen atom, in the presence of a base.
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- Substituted-(hydroxyphenyl)-pyrrolidine-2,5-dione stabilizers
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Substituted-(hydroxyphenyl)-pyrrolidine-2,5-dione derivatives of the formula STR1 are prepared by the reaction of the appropriate maleimide and phenolic compounds and are useful as stabilizers for organic polymers.
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- Preparation of pyrrolo[3,4-c]pyrroles
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A process for the preparation of 1,4-diketopyrrolo-[3,4-c]pyrroles of the formula STR1 wherein each of R1 and R2 independently of the other is an isocyclic or heterocyclic aromatic radical, which process comprises reacting 1 mole of a disuccinate with 2 moles of a nitrile of the formula or or with 1 mole of a nitrile of the formula (II) and 1 mole of the nitrile of the formula (III), in an organic solvent and in the presence of a strong base at elevated temperature, and obtaining the compound of formula I from the reaction product by hydrolysis. The pyrrolo-[3,4-c]pyrroles are suitable for pigmenting organic material of high molecular weight.
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- Process for the isomerization of isolated double bonds to conjugated double bonds in low-molecular weight homo- and/or copolymers of 1,3-dienes
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A process for the isomerization of isolated double bonds to conjugated double bonds in low-molecular weight homo- and/or copolymers of 1,3-dienes uses an isomerization catalyst optionally in the presence of a solvent, wherein the isomerization catalyst is a mixture of (a) a hydroxide of the alkali metals potassium, rubidium, or cesium, and an alcohol or (b) a lithium alcoholate or sodium alcoholate and a potassium, rubidium, or cesium salt or (c) sodium hydroxide, an alcohol, and a polar, aprotic compound. The isomerization is conducted at a temperature of 80°-220° C.
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- N-Alkoxy-N-acylnitrenium Ions as Possible Intermediates in Intramolecular Aromatic Substitution: Novel Formation of N-Acyl-3,4-dihydro-1H-2,1-benzoxazines and N-Acyl-4,5-dihydro-1H,3H-2,1-benzoxazepine
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N-Halogeno-N-alkoxyamides undergo intramolecular aromatic substitution by thermal- or Lewis acid-catalysed heterolysis of the nitrogen-halogen bond.N-Acyl-N-alkoxynitrenium ions are likely intermediates.N-Chloro-N-methoxybiphenyl-2-carboxamide (4) yields N-methoxyphenanthridone (11) quantitatively with AgBF4, while O-2-phenylethyl-N-chlorobenzohydroxamate (19) is converted in good yield into N-benzoyl-3,4-dihydro-1H-2,1-benzoxazine (21) with AgBF4, AgClO4, HgO, and Hg(OAc)2.N-Acetyl-3,4-dihydro-1H-2,1-bezoxazine (22) is formed similarly.O-3-Phenylpropyl-N-chlorobenzohydroxamate (23) cyclises to N-benzoyl-4,5-dihydro-1H,3H-2,1-benzoxazepine (24) with AgBF4.
- Glover, Stephen A.,Goosen, Andre,McCleland, Cedric W.,Schoonraad, Johan L.
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p. 2255 - 2260
(2007/10/02)
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- Process for preparing high cis 3-(2,2,2-trichloroethyl)-2,2-dimethylcyclopropane-1-carboxylates
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A process is described whereby esters of 3-(2,2,2-trichloroethyl)-2,2-dimethylcyclopropane-1-carboxylic acid are prepared predominantly in their cis isomer form. The process comprises treating a 4,6,6,6-tetrachloro-3,3-dimethylhexanoate with an alkali metal tert-alkoxide under controlled conditions of temperature in the presence of a defined solvent-cosolvent mixture. The products of the process are intermediates in the production of pyrethroid insecticides.
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- 5-Phenyl-thiazolidin-4-one derivatives
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The present invention is concerned with new pharmacologically effective 5-phenyl-thiazolidin-4-one derivatives and with the preparation thereof. These compounds are useful for treating liver dysfunctions.
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