HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 136390993, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 67291144 | HCID 67291144 | — |
| Solvent | Water ethanol | HCID 19096565 | — |
| Product | HCID 136390993 | HCID 136390993 | 101.9% |
Reaction Steps
A mixture of 3-(2,2,2-trifluoroethoxy)-6,7-dihydroquinolin-8(5H)-one (155 mg, 0.63 mmol), hydroxylamine hydrochloride (88 mg, 1.3 mmol), and sodium acetate (104 mg, 1.3 mmol) in ethanol-water (3:1, 4 mL) was refluxed with stirring for 2 hours. After cooling to room temperature, the mixture was poured into water, and the aqueous layer was extracted with dichloromethane (twice). The combined organic layers were dried over Magnesium sulfate and concentrated in vacuo to give 167 mg of the crude title compound as a brown solid. This was used for the next step without purification:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09101616B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-8878481d891447ecbfb5f04899259dc7 |
| Source note | uspto-grants-2015_08 |