Hydroxylamine → HCID 178482802, compound

HRID 2113902Notes

Reaction equation

HRID 2113902 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]=1

Participants

4

Reactant 2

HCID 787Hydroxylamine2×HCID 185261716-(Dimethylamino)pyridine-3-carbonitrile

Product 1

HCID 178482802HCID 178482802, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

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

  1. customThis mixture is reacted at 90° C. for 6 h
  2. temperaturethe mixture is cooled
  3. 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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