Nitric Acid → HCID 10967625, compound

HRID 744983Notes

Reaction equation

HRID 744983 reaction equation
[N+:1]([O-:4])(O)=[O:2].S(=O)(=O)(O)O.[Cl:10][C:11]1[C:21]([Cl:22])=[CH:20][C:14]2[O:15][C:16]([F:19])([F:18])[O:17][C:13]=2[CH:12]=1>>[Cl:22][C:21]1[C:11]([Cl:10])=[CH:12][C:13]2[O:17][C:16]([F:19])([F:18])[O:15][C:14]=2[C:20]=1[N+:1]([O-:4])=[O:2]

Participants

4

Reactant 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 11009682HCID 11009682, compound

Product 1

HCID 10967625HCID 10967625, compoundYield 89%

Procedure

A precooled mixture of 140 ml of 100% strength nitric acid and 200 ml of 100% strength sulphuric acid is added dropwise at 5° to 10° C. (internal temperature) with good stirring to 219 g (0.96 mol) of 5,6-dichloro-2,2-difluorobenzo[1.3]dioxole. The reaction mixture is then subsequently stirred at room temperature for 6 h. It is added to ice-water and extracted with ether, and the extract is dried and concentrated. 233 g (89% of theory) of 5,6-dichloro-4-nitro-2,2-difluoro-benzo(1.3)dioxole having a melting point of 29°-30° C. are obtained.

Workup

  1. additionis added dropwise at 5° to 10° C. (internal temperature)
  2. extractionextracted with ether
  3. customthe extract is dried
  4. concentrationconcentrated

Sources & evidence

ORD record
ord-76affa8f5fc84e03ad10e101ec03df13
Source dataset
uspto-grants-1996_09
Patent number
US05559253

Reaction notes

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