Nitric Acid → HCID 21459008, compound

HRID 725394Notes

Reaction equation

HRID 725394 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-2782568bf41344d594c261e8e45799cd
Source dataset
uspto-grants-1998_01
Patent number
US05705703

Reaction notes

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