Nitric Acid → HCID 21459008, compound

HRID 274526Notes

Reaction equation

HRID 274526 reaction equation
[N+:1]([O-:4])(O)=[O:2].[OH:5][C:6]1[CH:23]=[CH:22][C:9]([C:10]([C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][CH:13]=2)=[O:11])=[CH:8][C:7]=1[O:24][CH3:25]>>[OH:5][C:6]1[C:23]([N+:1]([O-:4])=[O:2])=[CH:22][C:9]([C:10]([C:12]2[CH:13]=[CH:14][C:15]([C:18]([F:20])([F:21])[F:19])=[CH:16][CH:17]=2)=[O:11])=[CH:8][C:7]=1[O:24][CH3:25]

Participants

3

Reactant 2

HCID 944Nitric AcidHCID 21459022HCID 21459022, compound

Product 1

HCID 21459008HCID 21459008, compound

Procedure

3.2 ml of 65 percent nitric acid are added dropwise within 10 minutes at 20° to 12.8 g of 4-hydroxy-3-methoxy-4'-(trifluoromethyl)benzophenone (dissolved in 160 ml of acetic acid). After stirring for 1.5 hours, the reaction mixture is poured into 600 ml of ice-water and the precipitate formed is filtered off, washed with water and dissolved in methylene chloride. The methylene chloride solution is dried over sodium sulfate and evaporated, and the residue is recrystallized from methylene chloride/hexane. There is obtained 4-hydroxy-3-methoxy-5-nitro-4'-(trifluoromethyl)benzophenone of melting point 172°.

Workup

  1. customthe precipitate formed
  2. filtrationis filtered off
  3. washwashed with water
  4. dissolutiondissolved in methylene chloride
  5. dry with materialThe methylene chloride solution is dried over sodium sulfate
  6. customevaporated
  7. customthe residue is recrystallized from methylene chloride/hexane

Sources & evidence

ORD record
ord-17385f10eb6241399b64064554a12bda
Source dataset
uspto-grants-1995_02
Patent number
US05389653

Reaction notes

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