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2-Chloronicotinonitrile → 2-Chloro-N'-hydroxynicotinimidamide

HRID 2415762
Notes
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Reaction equation

HRID 2415762 reaction equation
C[O-].[Na+].Cl.[NH2:5][OH:6].[Cl:7][C:8]1[C:13]([C:14]#[N:15])=[CH:12][CH:11]=[CH:10][N:9]=1>CO>[Cl:7][C:8]1[C:13]([C:14](=[N:5][OH:6])[NH2:15])=[CH:12][CH:11]=[CH:10][N:9]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 810792-ChloronicotinonitrileHCID 443297Hydroxyamine hydrochlorideHCID 10942334Sodium Methoxide

Product 1

HCID 406339952-Chloro-N'-hydroxynicotinimidamideYield 100.1%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Sodium methoxide (150 mi of 0.25M solution in methanol, 37.5 mmol) was added to a solution of hydroxylamine hydrochloride (2.8 g, 39.7 mmol) in methanol (150 mL), and the reaction was stirred at room temperature for 30 minutes. The mixture was filtered, then 2-chloro-3-cyanopyridine (5.0 g, 36.1 mmol) was added, the reaction was stirred at room temperature for 16 hours and then heated to reflux for 2 hours. The reaction was cooled to room temperature, concentrated in vacuo to approximately 50 mL and filtered. The filtrate was concentrated to dryness in vacuo, the residue was triturated with dichloromethane and filtered to give the title compound as a white solid (6.2 g).

Workup

  1. filtrationThe mixture was filtered
  2. stirringthe reaction was stirred at room temperature for 16 hours
  3. temperatureheated
  4. temperatureto reflux for 2 hours
  5. temperatureThe reaction was cooled to room temperature
  6. concentrationconcentrated in vacuo to approximately 50 mL
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated to dryness in vacuo
  9. customthe residue was triturated with dichloromethane
  10. filtrationfiltered

Sources & evidence

ORD record
ord-92c9310b65c64afaa27b14d92b4dd2c6
Source dataset
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06821972B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes