HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Hydroxide → HCID 178515628, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Ethyl 3-(4-iodophenyl)propiolate | HCID 66800188 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178515628 | HCID 178515628 | 57.1% |
Reaction Steps
To a solution of ethyl 3-(4-iodophenyl)propiolate (420 mg, 1.39 mmol) in MeOH (10 mL), were added hydroxylamine hydrochloride (391 mg, 5.20 mmol) and KOH (5 M in methanol, 1.7 mL, 8.5 mmol). The mixture was stirred at room temperature overnight and then concentrated in vacuo. The residue was redissolved in water (15 mL) and acidified with 2 M aqueous HCl to pH 2˜3. The precipitate was collected by filtration to afford the title compound (228 mg, 57%). 1H NMR (DMSO-d6, 400 MHz): δ 11.51 (brs, 1H), 7.94 (d, 2H), 7.65 (d, 2H), 6.67 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09399646B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-086402469f56452c80b015500ec38e03 |
| Source note | uspto-grants-2016_07 |