HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 178491837, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | 2,6-Difluoro-3-methoxybenzonitrile | HCID 3791832 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178491837 | HCID 178491837 | 43.6% |
Reaction Steps
To a solution of 2,6-difluoro-3-methoxybenzonitrile (0.30 g, 1.70 mmol) in EtOH (10 ml) was added hydroxylamine hydrochloride (0.12 g, 1.70 mmol) and NaOH (0.071 g, 1.70 mmol). The resulting reaction mixture was refluxed for 15 h. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added EtOH and filtered. The filtrate was evaporated in vacuo and the crude residue was purified over silica gel (60-120 M, 30% EtOAc-Hexane) to get the desired product (0.15 g, 42%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08415383B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-4b8a3b32071b4f4ba96b0764b952141f |
| Source note | uspto-grants-2013_04 |