Hydroxylamine → HCID 178482802, compound
Reaction equation
[CH3:1][N:2]([CH3:11])[C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[CH:5][N:4]=1.[NH2:12][OH:13]>C(O)C>[CH3:1][N:2]([CH3:11])[C:3]1[CH:10]=[CH:9][C:6]([C:7]([NH:12][OH:13])=[NH:8])=[CH:5][N:4]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
In a 100 ml round flask, 4.7 g (31.9 mmol) of 6dimethylamino-nicotinonitrile and 1.88 ml (31.9 mmol) of aqueous hydroxylamine (50%) are dissolved in 25 ml of ethanol. This mixture is reacted at 90° C. for 6 h. Then another 0.45 ml (8.1 mmol, 0.25 eq.) of hydroxylamine-solution is added. After 11 h at 90° C., the mixture is cooled and the solvent removed in vacuo. This yields the title compound as light yellow solid, which is used for the next step without purification. Mass spectrum: m/z (M+H)+: 181.0
Workup
- customThis mixture is reacted at 90° C. for 6 h
- temperaturethe mixture is cooled
- customthe solvent removed in vacuo
Sources & evidence
- ORD record
- ord-b201e66ae34b4d6b9f6b13973fe14b75
- Source dataset
- uspto-grants-2008_10
- Patent number
- US07432293B2
Reaction notes
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