Water → HCID 178510798, compound
Reaction equation
[C:1]1([CH2:7][C:8]#[N:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[NH2:11][OH:12].C(=O)([O-])[O-].[Na+].[Na+].O>CO>[OH:12][NH:11][C:8](=[NH:9])[CH2:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Procedure
Phenyl acetonitrile (20 g, 170 mmol), hydroxylamine hydrochloride (60 g, 850 mmol) and sodium carbonate (71 g, 850 mmol) were heated under reflux in methanol (300 ml) and water (300 ml) for 5 hours. The reaction mixture was cooled to room temperature, filtered and the filtrate was evaporated and extracted with dichloromethane (3×). The combined organic solutions were washed with water and brine, dried (MgSO4), filtered and concentrated under reduced pressure to give the title compound as a white solid, 15.5 g.
Workup
- filtrationfiltered
- customthe filtrate was evaporated
- extractionextracted with dichloromethane (3×)
- washThe combined organic solutions were washed with water and brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
Sources & evidence
- ORD record
- ord-a24aabb663e940d2b0ae35c01025435c
- Source dataset
- uspto-grants-2007_05
- Patent number
- US07217714B1
Reaction notes
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