HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxylamine HCl → HCID 73455958, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxylamine HCl | HCID 21645 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 1-(2,6-Dimethylphenyl)-2,2,2-trifluoroethan-1-one | HCID 18674537 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 73455958 | HCID 73455958 | 88.4% |
Reaction Steps
12.6 g (0.062 mol) of 2,2,2-trifluoro-1-(2,6-dimethylphenyl)-ethanone are dissolved in 30 ml of ethanol at 80° C. To the solution are added dropwise 4.6 g (0.066 mol) of hydroxylammonium chloride and 8.7 g (0.106 mol) of sodium acetate dissolved in 15 ml of water. The reaction mixture is refluxed overnight, affording white precipitation. The mixture is poured into ice water, and extracted with ethyl acetate. The organic phase is washed with water, NH4Cl aq, and brine, dried over MgSO4, and concentrated, yielding 11.9 g of crude 2,2,2-trifluoro-1-(2,4-dimethylphenyl)-ethanone oxime as a colorless liquid. The crude product is used in the next reaction step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06512020B1 |
| Source dataset | uspto-grants-2003_01 |
| ORD ID | ord-7c0bee1dc5584a8593ed51b729c955da |
| Source note | uspto-grants-2003_01 |