30-05-2019 дата публикации
Номер: US20190161452A1
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Process for the preparation of azidoperfluoroalkanes and azidopolyfluoroalkanes of general formula R—N, where Ris chosen from a group containing CF, CFH, CFXor RCFCF, where n is an integer in the range of 1 to 10, x is an integer in the range of 2 to 20, X is Cl, Br, or I, Ris Calkyl, ArO, ArS, imidazolyl, benzimidazolyl, or pyrazolyl and Ar is phenyl or substituted phenyl, by the reaction of electrophilic azidation reagent of general formula R—N, where Ris n-CFSO, ArSO, Br, I, with synthetic equivalent of polyfluoroalkylated carbanion of general formula [R]. 1: A method for preparation of azidoperfluoroalkanes and azidopolyfluoroalkanes of formula R—N ,{'sub': F', 'n', '2n+1', 'n', 'x', '2n+1−x', 'n', 'x', '2n+1−x', '2', '2, 'sup': '1', 'wherein Ris selected from the group consisting of CF, CFH, CFXor RCFCF, wherein n is an integer in the interval from 1 to 10, x is an integer in the interval from 2 to 20 and'}X is Cl, Br, or I,{'sup': '1', 'sub': '1-10', 'Ris selected from the group consisting of Calkyl, ArO, ArS, imidazolyl, benzimidazolyl, or pyrazolyl and Ar is phenyl or substituted phenyl,'}said process having the following steps{'sub': 'F', 'sup': '−', '(A) generation of a synthetic equivalent of polyfluoroalkyl carbanion, said synthetic equivalent having the formula [R], by a method selected from{'sup': 3', '3, 'sub': 3', 'F', '1-5, 'a) activation of trialkyl(polyfluoroalkyl)silane of general formula RSiR, wherein Ris Calkyl, with a Lewis base which is selected from the group consisting of potassium fluoride, cesium fluoride, tetramethylammonium fluoride, tetrabutylammonium fluoride, sodium carbonate, potassium carbonate, potassium phosphate, sodium acetate, potassium acetate, tetrabutylammonium acetate;'}{'sub': F', '1-5, 'sup': 3', '3, 'b) reaction of polyfluoroalkane of general formula RH with a base which is selected from a group consisting of methyllithium, butyllithium, phenyllithium, Grignard reagent of general formula RMgX, wherein Ris Calkyl, and ...
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