Hydrogen Peroxide → HCID 10352010, compound
Reaction equation
[F:1][C:2]([F:10])([F:9])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.[OH:11]O>C(O)(=O)C>[F:1][C:2]([F:10])([F:9])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N+:4]=1[O-:11]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 70 °C
Procedure
To a stirred solution of 2-trifluoromethyl pyridine (5 g, 34 mmol) in acetic acid (25 mL) is added 33% of aqueous H2O2 (20 mL) at room temperature. The reaction mixture is allowed to stir for 12 h at 70° C. After complete consumption of starting material the reaction mixture is concentrated under reduced pressure. The residue is dissolved in chloroform (250 mL) and pH is adjusted to 7 with K2CO3 (20 g approx). Resulting solid is filtered through glass sintered funnel and washed with chloroform. Filtrate is concentrated under reduced pressure to give 2-trifluoromethyl-pyridine 1-oxide as syrupy liquid (4.3 g).
Workup
- customAfter complete consumption of starting material the reaction mixture
- concentrationis concentrated under reduced pressure
- dissolutionThe residue is dissolved in chloroform (250 mL)
- customResulting solid
- filtrationis filtered through glass sintered funnel
- washwashed with chloroform
- concentrationFiltrate is concentrated under reduced pressure
Sources & evidence
- ORD record
- ord-595de53777d74446aa43ab85662dfa98
- Source dataset
- uspto-grants-2013_01
- Patent number
- US08362249B2
Reaction notes
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