Nitric Acid → HCID 22910002, compound

HRID 744984Notes

Reaction equation

HRID 744984 reaction equation
[N+:1]([O-:4])(O)=[O:2].S(=O)(=O)(O)O.[Br:10][C:11]1[C:24]([Br:25])=[CH:23][C:14]2[O:15][C:16]([F:22])([F:21])[C:17]([F:20])([F:19])[O:18][C:13]=2[CH:12]=1>>[Br:25][C:24]1[C:11]([Br:10])=[CH:12][C:13]2[O:18][C:17]([F:20])([F:19])[C:16]([F:21])([F:22])[O:15][C:14]=2[C:23]=1[N+:1]([O-:4])=[O:2]

Participants

4

Reactant 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 22910004HCID 22910004, compound

Product 1

HCID 22910002HCID 22910002, compoundYield 88%

Conditions

Temperature
5 °C

Procedure

A precooled mixture of 19 ml of nitric acid and 26 ml of concentrated sulphuric acid is slowly added dropwise at 5° C. to 73 g (0.2 mol) of 6,7-dibromo-2,2,3,3-tetrafluoro-benzo(1.4)dioxane. The mixture is subsequently stirred at 5° C. for 4 hours, poured onto ice and extracted thoroughly with ether, the extract is washed with water and sodium hydrogen carbonate solution (until neutral), and dried over magnesium sulphate, and the ether is removed. 72 g (88% of theory) of 6,7-dibromo-5-nitro-2,2,3,3-tetrafluoro-benzo(1.4)dioxane having the melting point 91° to 92° C. are isolated.

Workup

  1. additionpoured onto ice
  2. extractionextracted thoroughly with ether
  3. washthe extract is washed with water and sodium hydrogen carbonate solution (until neutral)
  4. dry with materialdried over magnesium sulphate
  5. customthe ether is removed

Sources & evidence

ORD record
ord-a2bb3cac8ede4a3eac7c5cf5e8342e2a
Source dataset
uspto-grants-1996_09
Patent number
US05559253

Reaction notes

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