Azobisisobutyronitrile → HCID 89690256, compound
Reaction equation
[CH3:1][C:2]1[CH:7]=[N:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][N:3]=1.[Br:12]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>FC(C1C=CC=CC=1)(F)F>[Br:12][CH2:1][C:2]1[CH:7]=[N:6][C:5]([C:8]([F:11])([F:9])[F:10])=[CH:4][N:3]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 90 °C
Procedure
To a solution of 2-methyl-5-(trifluoromethyl)pyrazine (1 g) in trifluoromethylbenzene (10 ml) was added N-bromosuccinimide (1.21 g) at room temperature, and the mixture to was stirred at 90° C. for 30 min. To the obtained reaction mixture was added azobisisobutyronitrile (0.051 g), and the mixture was stirred at the same temperature for 7 hr. The reaction mixture was cooled and concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (404 mg).
Workup
- customTo the obtained reaction mixture
- stirringthe mixture was stirred at the same temperature for 7 hr
- temperatureThe reaction mixture was cooled
- concentrationconcentrated under reduced pressure
- customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate)
Sources & evidence
- ORD record
- ord-9d47bf77254d48549b00eb083021371a
- Source dataset
- uspto-grants-2015_12
- Patent number
- US09199963B2
Reaction notes
Loading…