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ChemicalBook CAS DataBase List 2,4,4,6-TETRABROMO-2,5-CYCLOHEXADIENONE

2,4,4,6-TETRABROMO-2,5-CYCLOHEXADIENONE synthesis

13synthesis methods
-

Yield:20244-61-5 94%

Reaction Conditions:

with sodium bromate;oxalic acid;sodium bromide in water for 8.16667 h;

Steps:

4 EXAMPLE-4
To a well stirred solution of 5.00 g (53 mmoles) of phenol, 15.00 g (145 mmoles) of sodium bromide and 10.93 g (72 mmoles) of sodium bromate in 100 ML of deionized water in a 250 ml round bottom flask, was slowly added a solution of 27.72 g (220 mmoles) of oxalic acid dihydrate in 50 ML water over 10 min.The contents were stirred for another 8 h.The precipitated product was filtered, washed twice with deionized water and dried in vacuum for 6 h.The total crude yield of 2,4,4,6-tetrabromo-2,5-cyclohexadienone was 20.5 g (94%) which melted at 123 degree C.; IR (KBr) υ 634, 663, 702, 900, 1310, 1454, 1582, 1680, 3051 cm-1; 1H-NMR (CDCl3, 200 MHz) δ 7.78 (s, 2H) and elemental analysis, observed 17.16 (% C) 0.24 (% H), calculated for C6H2Br4O; 17.56 (% C) 0.49 (% H).

References:

Council of Scientific and Industrial Research US2004/127750, 2004, A1 Location in patent:Page 3

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