Nitric Acid → HCID 20461931, compound

HRID 326030Notes

Reaction equation

HRID 326030 reaction equation
[N+:1]([O-:4])(O)=[O:2].[F:5][CH:6]([F:18])[O:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH:15]([F:17])[F:16])=[CH:10][CH:9]=1>ClCCCl>[F:5][CH:6]([F:18])[O:7][C:8]1[CH:9]=[CH:10][C:11]([O:14][CH:15]([F:17])[F:16])=[CH:12][C:13]=1[N+:1]([O-:4])=[O:2]

Participants

4

Reactant 2

HCID 944Nitric AcidHCID 133315561,4-Bis(difluoromethoxy)benzene

Product 1

HCID 20461931HCID 20461931, compound

Reagents, catalysts & solvents 1

HCID 111,2-DichloroethaneSolvent

Conditions

Temperature
5 °C

Procedure

10 ml of nitric acid (100%) are added dropwise at a temperature of -5° to 0° C. within 5 minutes to a solution of 13.9 g of 1.4-bis(difluoromethoxy)benzene in 33 ml of 1.2-dichloroethane. The reaction mixture is stirred for a further hour at a temperature of 5° C. and allowed to warm to 15° C. within 1/2 hour. The mixture is then poured into icewater. The organic phase is separated, washed with 10% aqueous sodium hydroxide solution, dried over sodium sulfate and evaporated to dreyness, yielding 12.6 g of crude 2.5-bis(difluoromethoxy)-nitrobenzene in form of a yellowish oil.

Workup

  1. temperatureto warm to 15° C. within 1/2 hour
  2. additionThe mixture is then poured into icewater
  3. customThe organic phase is separated
  4. washwashed with 10% aqueous sodium hydroxide solution
  5. dry with materialdried over sodium sulfate
  6. customevaporated to dreyness

Sources & evidence

ORD record
ord-3a00263d3bb246bdb2f6d22b26866595
Source dataset
uspto-grants-1984_04
Patent number
US04444583

Reaction notes

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