HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 1-(3-Amino-4-hydroxyphenyl)ethanone O-methyloxime
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | HCID 59444173 | HCID 59444173 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 1-(3-Amino-4-hydroxyphenyl)ethanone O-methyloxime | HCID 136337192 | — |
Reaction Steps
A mixture of O-methylhydroxylamine hydrochloride (535 mg, 6.40 mmol), 2-amino-4-(2-methyl-1,3-dioxolan-2-yl)phenol D130 (250 mg, 1.28 mmol) and potassium carbonate (442 mg, 3.20 mmol) in ethanol (10 mL) was heated to reflux for 2 hr. The mixture was cooled to rt and concentrated to dryness under vacuum and the residue partitioned between DCM and water. The organic phase was separated washed with brine, dried (MgSO4) and concentrated to dryness in vacuo. The residue was purified using silica gel chromatography eluting with 0 to 10% MeOH in DCM. The title product was isolated as a pale brown solid, 224 mg, 97%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08278328B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-e206473a9d854fdc9735eef39cc3e926 |
| Source note | uspto-grants-2012_10 |