HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 136349114, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | HCID 12462879 | HCID 12462879 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 136349114 | HCID 136349114 | — |
Reaction Steps
The product from Example 16A (479 mg, 2.06 mmol), methoxylamine hydrochloride (275 mg, 3.29 mmol), and pyridine (0.36 mL, 4.45 mmol) were stirred in methanol (5 mL) at room temperature overnight. After this time, the solvent was evaporated in vacuo, and the residue was taken up in ethyl acetate and washed with 1N HCl and brine. The organic solution was dried over Na2SO4 and was evaporated in vacuo. Chromatography on silica gel (4:1 hexane-ethyl acetate, eluant) afforded the title compound as a colorless oil, 524 mg (97%). 1H NMR (300 MHz, DMSO-d6) δ 9.79 (br, 1H), 7.54 (d, J=8.8 Hz, 1H), 6.35 (m, 1H), 6.22 (m, 1H), 3.84 (s, 3H), 2.68 (s, 2H), 1.25-1.79 (m, 10H). MS (DCI+) m/z 262 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598220B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-8b32d042f1a247f698eda62254d1b498 |
| Source note | uspto-grants-2013_12 |