Nitric Acid → HCID 21226452, compound

HRID 583047Notes

Reaction equation

HRID 583047 reaction equation
[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=2)=[N:4][N:5]([CH3:11])[C:6]=1[O:7][CH:8]([F:10])[F:9].[N+:19]([O-])([OH:21])=[O:20]>>[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([N+:19]([O-:21])=[O:20])[CH:13]=2)=[N:4][N:5]([CH3:11])[C:6]=1[O:7][CH:8]([F:9])[F:10]

Participants

3

Reactant 2

HCID 944Nitric AcidHCID 15220185HCID 15220185, compound

Product 1

HCID 21226452HCID 21226452, compound

Procedure

113.4 g (0.387 mol) of 4-chloro-3-(4-chlorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole were added a little at a time at -40° C. to 500 ml of 98% strength nitric acid. The mixture was stirred at this temperature for 2 hours and then the solution was stirred into ice. The product was extracted from the aqueous phase with dichloromethane. The dichloromethane phase was subsequently washed a number of times with water and then with saturated sodium chloride solution. Drying over magnesium sulfate and removal of the dichloromethane gave 119.6 g of the target product.

Workup

  1. stirringthe solution was stirred into ice
  2. extractionThe product was extracted from the aqueous phase with dichloromethane
  3. washThe dichloromethane phase was subsequently washed a number of times with water
  4. dry with materialDrying over magnesium sulfate and removal of the dichloromethane

Sources & evidence

ORD record
ord-7e961b1db0ed4cddbc536387d7de26b7
Source dataset
uspto-grants-1999_07
Patent number
US05928999

Reaction notes

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