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A process for producing 2,3,4,5-tetrafluorobenzoYlfluoride and 2,3,4,5-tetrafluorobenzoTrifluoride

机译:制备2,3,4,5-四氟苯并三氟甲苯和2,3,4,5-四氟苯并三氟甲苯的方法

摘要

A process for producing 2,3,4,5-tetrafluorobenzoylfluoride and 2,3,4,5-tetrafluorobenzotrifluoride, important intermediate products in the synthesis of medicaments, by an interaction of 2,3,4,5-tetrachlorobenzoylchloride (2,3,4,5-tetrachlorobenzotrifluoride) with potassium fluoride in the absence of dissolvent in two stages at the temperature of 160-205оС in the presence of catalyst of the general formula EMBED ISISServer , wherein R1-R4 = СН3-С21Н43, С6Н5; R1=R2=R3=R4 or R1 EMBED Equation.3 R2 EMBED Equation.3 R3 EMBED Equation.3 R4; Х = Сl, Вr, I, РО EMBED Equation.3 , SO EMBED Equation.3 , СО EMBED Equation.3 , СН3СОO-, and cocatalyst - one of the following organic compounds: freon-11, freon-12, freon-112, freon-113, dimethylformamide, N-methylpyrrolidone, dimethylacetamide, dimethylsulfoxide, dialkyl ethers, chloroform, methylenechloride, monoglyme, diglyme, hexametalol, hexaethylphosphorotriamide, acetonitrile, dioxane, pentafluorethane, perfluoralkanes, tetrahydrofuran at the molar ratio of components equal to 2,3,4,5-tetrachlorobenzoylchloride or 2,3,4,5-tetrachlorobenzotrifluoride:catalyst: cocatalyst = 1:(0,01-0,1):(0,01-0,02) respectively. These conditions provide for output of objective substances between 75 % and 87 % with a possibility of regeneration of catalyst at the first stage of fluorination, reducing reaction temperature by 20-30oC and exclusion of use of expensive dissolvent - sulfolane.
机译:一种通过2,3,4,5-四氯苯甲酰氯的相互作用生产2,3,4,5-四氟苯甲酰氟和2,3,4,5-四氟苯甲酰氟的方法,这些中间体是药物合成中的重要中间产物(2,3在通式为EMBED ISISServer的催化剂存在下,在160-205℃下在不存在溶剂的情况下在两个阶段中在不存在溶剂的情况下用氟化钾制备(4,5-四氯苯并三氟化物),其中R1-R4 =С3-3-212143,С6Н5; R1 = R2 = R3 = R4或R1 EMBED公式3 R2 EMBED公式3 R3 EMBED公式3 R4; Х=Сl,Вr,I,РОEMBED Equation.3,SO EMBED Equation.3,СОEMBED Equation.3,СН3СОO-和助催化剂-以下有机化合物之一:氟利昂11,氟利昂12,氟利昂112 ,氟利昂113,二甲基甲酰胺,N-甲基吡咯烷酮,二甲基乙酰胺,二甲基亚砜,二烷基醚,氯仿,二氯甲烷,一甘醇二甲醚,二甘醇二甲醚,六金属醇,六乙基磷三酰胺,乙腈,二恶烷,五氟乙烷,全氟烷烃,四氢呋喃1,4,5-四氯苯甲酰氯或2,3,4,5-四氯苯甲酰氟:催化剂:助催化剂= 1:(0.01,0.1):( 0.01-0,02)。这些条件使目标物质的输出量介于75%至87%之间,并有可能在氟化的第一阶段使催化剂再生,将反应温度降低20-30oC,并且不使用昂贵的溶剂-环丁砜。

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