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ChemicalBook CAS DataBase List Bromopentafluorobenzene
344-04-7

Bromopentafluorobenzene synthesis

11synthesis methods

To 250mL four-necked bottle add 208g trichloromethane, 38.5g bromine (0.24mol), lowering the temperature to -5 ° C, through 17g chlorine (0.24mol), the resulting chlorinated bromine trichloromethane solution at 35 ° C dropwise added to the reaction ket

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Yield:344-04-7 93%

Reaction Conditions:

with tris(pentafluorophenyl)borate;bromine;chlorine in chloroform at 30 - 35; for 2 h;Large scale;Reagent/catalyst;Solvent;Temperature;

Steps:

1-7 Example 6

Add 3.125 kg of chloroform to a 3L four-necked flask. 0.574 kg of bromine (3.59 mol), Cool down to -5 ° C, Passing 0.255kg of chlorine (3.59mol), The obtained chlorobromide solution in chloroform was added dropwise at 30-35 ° C to a reaction vessel containing 1.208 kg of pentafluorobenzene (7.19 mol) and 0.109 kg of tris(pentafluorophenyl)borane(0.22 mol). Stirring for 2 hours (detecting complete conversion of reaction materials, 0.04% of pentafluorochlorobenzene impurities), after post-treatment, After removing the solvent by distillation under reduced pressure, Reduced distillation to obtain 1.650kg of pentafluorobromobenzene. Yield 93%, HPLC: 99.7% (main impurity pentafluorochlorobenzene, HPLC: 0.01%).

References:

CN109438168,2019,A Location in patent:Paragraph 0024-0037

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