Hydroxyamine hydrochloride → HCID 57368850, compound
Reaction equation
[Na].[NH2:2][OH:3].Cl.[F:5][C:6]([F:11])([F:10])[CH2:7][C:8]#[N:9]>CO>[F:5][C:6]([F:11])([F:10])[CH2:7][C:8](=[N:2][OH:3])[NH2:9]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
Into a flask containing sodium (45.87 mmol, 2.5 g) in MeOH (10 ml), a suspension of NH2OH.HCl (45.87 mmol, 3.2 g) in MeOH (11 ml) was added using a dropping funnel. After addition, the mixture was stirred for 15 min. The suspension was filtered to remove the precipitated NaCl. The filtrate was cooled to 0° C. and 3,3,3-trifluoropropionitrile (45.87 mmol, 5 g) was added. The reaction mixture was stirred for 1 h. The solvent was evaporated under reduced pressure. The crude product was proceeded to the next step without purification. Yield 3.0 g.
Workup
- additionwas added
- additionAfter addition
- filtrationThe suspension was filtered
- customto remove the precipitated NaCl
- stirringThe reaction mixture was stirred for 1 h
- customThe solvent was evaporated under reduced pressure
- customThe crude product was proceeded to the next step without purification
Sources & evidence
- ORD record
- ord-091b5b65cb544dc1842cdda11a91d07c
- Source dataset
- uspto-grants-2014_12
- Patent number
- US08921378B2
Reaction notes
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