Hydroxylamine → HCID 178513323, compound
Reaction equation
[F:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[NH2:10][OH:11]>C(O)C>[F:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]([NH:10][OH:11])=[NH:7])=[CH:4][CH:3]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 90 °C
Procedure
In a 50 ml round bottom flask, 3.0 g (24.8 mmol) of 4-fluoro-benzonitrile are suspended in 50 ml of ethanol and 1.46 ml of aqueous hydroxylamine (50%, 24.8 mmol) are added. The mixture is heated to 90° C. and the resulting solution stirred at this temperature for 16 h. After cooling to room temperature, the solvent is removed in vacuo and the resulting residue recrystallised from 25 ml of ethanol/water (1:5) which yields a white solid. Mass spectrum: m/z (M+H)+: 155.0
Workup
- temperatureAfter cooling to room temperature
- customthe solvent is removed in vacuo
- customthe resulting residue recrystallised from 25 ml of ethanol/water (1:5) which
- customyields a white solid
Sources & evidence
- ORD record
- ord-6adbb530c5f74ec4add330a92072f8c6
- Source dataset
- uspto-grants-2008_10
- Patent number
- US07432293B2
Reaction notes
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