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Method of obtaining 5- halogenalkyl-4,5-dihydroisoxazole derivatives Invention relates to a method of obtaining a compound of formula , where R1 represents CHX2, CX3, CX2CHX2 or CX2CX3; each X independently represents Cl or F; Z represents phenyl, optionally substituted with one or more substituents, independently selected from R2; and each R2 independently represents halogen, C1-C6 alkyl or C1-C6 halogenalkyl; Q represents Qb; Qb represents 1-naphthalenyl, optionally substituted with R3; each R3 independently represents halogen, C1-C6 alkyl, C1-C6 halogenalkyl, -C(=W)N(R4)R5 or-C(=W)OR5; each R4 represents H; each R5 represents H or C1-C6 alkyl, optionally substituted with R6; each R6 represents C2-C7 alkylaminocarbonyl or C2-C7 halogenalkylaminocarbonyl; and each W independently represents O; including the stage, at which a compound of formula , where R1, Q and Z are determined before for the formula 1 compound, contacts with hydroxylamine in the presence of a base. Hydroxylamine is obtained from the hydroxylamine salt. The base includes one or more compounds, selected from amine bases, hydroxide bases of alkali metals, alkoxide bases of alkali metals and carbonate bases of alkali metals. The invention also relates to the formula 2 compound, N-oxides and their salts, and such a particular compound as 4-acetyl-1-naphthalenecarbonyl chloride. |
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Method of obtaining meta-chlorobenzophenone as half-product of anticonvulsive medication "halodif" Meta-chlorobenzophenone is obtained by diazotization of 2-amino-5-chlorobenzophenone at room temperature. Diazotization is carried out in mixture of icy acetic and hydrochloric acids with application of water solution of sodium nitrate with the following processing of obtained salt of diazonium with water solution of sodium hypophosphite or copper protoxide in ethyl alcohol for 0.5-1 h. |
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Method of producing 3-trifluoromethyl chalcones Invention relates to an improved method of producing a compound of formula , where Z is optionally substituted phenyl and Q is phenyl or 1-naphthalenyl, each optionally substituted. The method involves distillation of water from a mixture containing a compound of formula , a compound of formula , a base containing at least one compound selected from a group comprising alkali-earth metal hydroxides of formula 4 M(OH)2, where M is Ca, Sr or Ba, alkali metal carbonates of formula 4a (M1)2CO3 , where M1 is Li, Na or K, 1,5-diazabicyclo[4,3.0]non-5-ene and 1,8-diazabicyclo[5.4.0]undec-7-ene, and an aprotic solvent capable of forming a low-boiling azeotrope with water. The invention also relates to a method of producing a compound of formula 2, a method of producing a compound of formula from a compound of formula 1 and a compound of formula 2. |
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Method of producing fluorine-containing tetraketones Present invention relates to a method of producing fluorine-containing tetraketones of general formula: , where I) R1=CHCH(CH3)2; R2=CH3; II)R1=CH2; R2=Ph III) R1=CHCH2CH3; R2=Ph, which can be used as synthons for producing their fluorine-containing aza- and thio-analogues, β-hydroxyketones, pyrazoles, isoxazoles, as well as biologically active substances. The method involves reacting a diester of perfluoro-dicarboxylic acid with an alkylketone in the presence of sodium hydride in the medium of an organic solvent. The diester of perfluoro-dicarboxylic acid used is dimethyl ester of perfluoro-dodecane dicarboxylic acid and the alkylketone used is: acetophenone, methyl isobutyl ketone or propyl phenyl ketone, and the process is carried out in the presence of a catalyst - dibenzo-24-crown-8 ester, in molar ratio diester of perfluoro-dicarboxylic acid: alkylketone: sodium hydride: catalyst equal to 1 : (2-3.5) : 1 : (0.00025-0.0005). |
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4,4'-difluorobenzophenone synthesis method Present invention relates to a method for synthesis of 4,4'-difluorobenzophenone, the main raw product for synthesis of aromatic polyester-ketones. The method involves a first step where fluorobenzene reacts with formaldehyde under conditions for catalysis with organic sulphonic acids to form difluorodiphenylmethane. The product is extracted and oxidised with nitric acid at the second step to 4,4'-difluorobenzophenone. |
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Method of producing m-chlorobenzophenone M-chlorobenzophenone is used as an intermediate product in synthesis of original anticonvulsant "halodif" (m-chlorobenzhydrylurea). The method involves diazotisation of 2-amino-5-chlorobenzophenone at room temperature using p-toluenesulfonic acid and polymer diazotising agent, with subsequent treatment of the obtained diazonium tosylate with an aqueous solution of sodium hypophosphite. |
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Production method for 1-(4-chlorophenyl)-2-cyclopropylpropane-1-one and by-product therefor Invention refers to production method of 1-(4-chlorophenyl)-2-cyclopropylpropane-1-one being a by-product for making biologically active substances, as well as to production method for 1-(4-chlorophenyl)-2-methyl-3-butene-1-one being a by-product for making 1-(4-chlorophenyl)-2-cyclopropylpropane-1-one. Production method for 1-(4-chlorophenyl)-2-cyclopropylpropane-1-one consists that 4-chlorobenzonitrile reacts with crotyl chloride or bromide and zinc in organic solvent and optionally with aluminium chloride. Hydrolysis of reaction mixture 2M with hydrochloric acid results in separation 1-(4-chlorophenyl)-2-methyl-3-butene-1-one thereafter purified. It reacts dibromomethane, zinc and copper monochloride in organic solvent with catalyst added or in ultrasonic bath. It is followed with separation of end product by common method. |
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Novel trifunctional photoinitiators Invention concerns new photoinitiators, method of their obtainment, compositions hardening with irradiation, and application of those compositions in coating preparation. Invention claims photoinitiators of formulae I , where R1, R2, R3 and R4 are independently C1-C8alkyl or benzyl; or R1 and R2 together and/or R3 andR4 together are cyclohexyl; R5 is hydrogen; A is OH, Br, -O-C1-C12alkyl, -O-R7, where R7 is linear or forked C2-C21hydroxyalkyl carbon chain interrupted by 1 to 9 oxygen atoms; or -NR8R9, where R8 and R9 are independently C1-C21alkyl or C2-C4alkyl substituted by one or more OH groups; A' is -O-; X and Y are independently -OH or -N(CH3)2; n is 2; R6 is linear or forked divalent -CO-NH-(C2-C16alkylene)-(NH-CO)- radical or linear or forked -CO-NH-(C0-C9alkylene)-(NH-CO)- which can be interrupted by phenylene, or linear or forked divalent -C2-C50alkylene radical with carbon chain interrupted by 1 to 15 oxygen atoms. |
Another patent 2551133.
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