Dimethylformamide → HCID 58336758, compound
Reaction equation
[CH3:1][C:2]1[N:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][CH:3]=1.[CH3:10][N:11]([CH:13]=O)[CH3:12]>>[CH3:10][N:11]([CH3:13])/[CH:12]=[CH:1]/[C:2]1[N:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][CH:3]=1Participants
3
Procedure
20 g (169 mmol) of 6-methylpyridine-2-carbonitrile were reacted in a mixture of in each case 100 ml of DMF and DMF-dimethyl acetal in an autoclave at 175° C. overnight. After cooling, the mixture was concentrated by evaporation, the residue was dissolved in dichloromethane, the solution was filtered, the filtrate was concentrated and the residue was subjected to distillation under reduced pressure in a kugelrohr.
Workup
- temperatureAfter cooling
- concentrationthe mixture was concentrated by evaporation
- dissolutionthe residue was dissolved in dichloromethane
- filtrationthe solution was filtered
- concentrationthe filtrate was concentrated
- distillationthe residue was subjected to distillation under reduced pressure in a kugelrohr
Sources & evidence
- ORD record
- ord-fb97567f473d429f8afd55f3c38d3726
- Source dataset
- uspto-grants-2014_04
- Patent number
- US08685964B2
Reaction notes
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