HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → 686347-58-0
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | 686345-96-0 | HCID 21905841 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 686347-58-0 | HCID 21905790 | — |
Reaction Steps
A mixture of 1-[9-(4-chlorophenyl)-8-(2-chlorophenyl)-9H-purin-6-yl]-piperidin-4-one 7A-96 (75 mg, 0.17 mmol) and hydroxylamine hydrochloride (11.9 mg, 0.17 mmol) in methanol (0.3 ml) was stirred overnight at room temperature. The reaction was then extracted from saturated aqueous sodium bicarbonate, the combined organic layers were dried (Na2SO4) and concentrated to afford title compound 32A-1 (75 mg, 97%) as a solid: +ESI MS (M+1) 453.4; 1H NMR (400 MHz, DMSO-d6) δ 10.49 (s, 1H), 8.28 (s, 1H), 7.70 (dd, J=7.7, 1.5 Hz, 1H), 7.53–7.41 (m, 5H), 7.31 (d, J=8.7 Hz, 2H), 4.45–4.18 (v br s, 4H), 2.61 (t, J=6.0 Hz, 2H), 2.39 (t, J=5.8 Hz, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07129239B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-5d685d758b6949e28adf06425086674d |
| Source note | uspto-grants-2006_10 |