HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxylamine HCl → HCID 73455956, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxylamine HCl | HCID 21645 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 3',4'-Dimethoxy-2,2,2-trifluoroacetophenone | HCID 2758493 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 73455956 | HCID 73455956 | 95.2% |
Reaction Steps
2.9 g (9.7 mmol) of 2,2,2-trifluoro-1-(3,4-dimethoxyphenyl)-ethanone are dissolved in 12 ml of ethanol at 80° C. To the solution are added dropwise 0.83 g (12.0 mmol) of hydroxylammonium chloride and 1.2 g (15.0 mmol) of sodium acetate dissolved in 6 ml of water. The reaction mixture is refluxed for 7.5 hours, poured into ice water, and extracted with ether. The organic phase is washed with water and brine, dried over MgSO4, and concentrated, yielding 2.3 g of 2,2,2-trifluoro-1-(3,4-dimethoxyphenyl)-ethanone oxime. 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-388b49e9ec0444ddb2708ebc37e73051 |
| Source note | uspto-grants-2003_01 |