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ChemicalBook CAS DataBase List 3,5-Difluorochlorobenzene
1435-43-4

3,5-Difluorochlorobenzene synthesis

9synthesis methods
-

Yield:372-38-3 74% ,1435-43-4 6.7%

Reaction Conditions:

with potassium fluoride;3-nitro-N,N-dimethylbenzamide;1,3-dimethyl-2-(N',N',N",N"-tetramethylguanidino)-4,5-dihydro-3H-imidazolium chloride in sulfolane at 220; under 6000.6 Torr; for 48 h;

Steps:

4
Example 4; Preparation method of 1,3,5-trifluorobenzene; 500 g of 1,3,5-trichlorobenzene, 1180 ml of sulpholane, 10.7 g of 3-nitrodimethylbenzamide and 640 g of dry KF were initially charged in an autoclave, then 48 g of CNC catalyst were added and the autoclave was sealed. The mixture was heated to 220° C. for 48 h. During the reaction, a maximum total pressure of 8 bar arose. Subsequently, the mixture was cooled to 20° C. The product was distilled off initially at standard pressure, later under reduced pressure. 310 g of a colourless liquid having a proportion of 87% by weight of 1,3,5-trifluorobenzene (74% of theory) and 8.8% by weight of difluorochlorobenzene (6.7% by weight of theory) were obtained. 1,3,5-Trifluorobenzene and difluorochlorobenzene can be separated distillatively in a known manner.

References:

Pleschke, Axel;Marhold, Albrecht US2006/9643, 2006, A1 Location in patent:Page/Page column 5

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