Hydroxyamine hydrochloride → HCID 57368850, compound

HRID 1409450Notes

Reaction equation

HRID 1409450 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

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

  1. additionwas added
  2. additionAfter addition
  3. filtrationThe suspension was filtered
  4. customto remove the precipitated NaCl
  5. stirringThe reaction mixture was stirred for 1 h
  6. customThe solvent was evaporated under reduced pressure
  7. 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

Loading…