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ChemicalBook CAS DataBase List 5-Bromo-1,2,3-trifluorobenzene
138526-69-9

5-Bromo-1,2,3-trifluorobenzene synthesis

13synthesis methods
-

Yield:138526-69-9 94.6%

Reaction Conditions:

with sodium hypochlorite;sodium dihydrogenphosphate;sodium bromide in dichloromethane;water at 8 - 15; for 2.66667 h;Temperature;

Steps:

1-3 Example 2
The preparation method of 3,4,5-trifluorobromobenzene is as follows:(1) Add 1 mol of 1,2,3-trifluorobenzene and 3 mol of dichloromethane to a 2 L reaction flask.Stir the solution into a solution and cool to 8-12 ° C;(2) dissolving 1.0 mol of sodium bromide and 120 g of sodium dihydrogen phosphate in water,Formulated into an aqueous solution, cooled to 12 ° C and added to the reaction bottle of step (1);(3) 10% sodium hypochlorite solution (1.2 mol sodium hypochlorite content) was added dropwise to the reaction flask at 15 ° C, the dropping process was carried out for 100 min, and the temperature reaction was maintained for 60 min;(4) After standing and phase separation, the organic phase is washed to neutral,Calcium chloride is dried and the organic phase is desolvated to obtain crude 3,4,5-trifluorobromobenzene;(5) melt recrystallization of crude 3,4,5-trifluorobromobenzene at -25 ° C,200 g of the product 3,4,5-trifluorobromobenzene were obtained in a yield of 94.6% and a content of 99.5%.

References:

Sinopharm Group Chemical Reagent Co., Ltd.;Gu Xiaoyan;Qin Jianguo;Ling Fang;Wu Xiaolan CN108947763, 2018, A Location in patent:Paragraph 0020-0040

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