化工社化工社 化学情報印刷レポート · 研究参考用
Hydroxylamine → Methyl 3-[amino(hydroxyimino)methyl]-4-methoxybenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxylamine | HCID 787 | — |
| 反応物 | Methyl 3-cyano-4-methoxybenzoate | HCID 2801011 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Methyl 3-[amino(hydroxyimino)methyl]-4-methoxybenzoate | HCID 53410613 | 98.7% |
反応手順
A solution of methyl 3-cyano-4-methoxybenzoate (518 mg, 2.71 mmol), hydroxylamine (810 μL, 50% in water, 13.55 mmol) in EtOH (20 mL) was heated for 18 h at 60° C. after which time solvents were removed under vacuum, solid residue was triturated with water filtered and dried under vacuum overnight to give the title compound as an off-white solid (600 mg, quant). 1H NMR (DMSO-d6, 300 MHz) δ 9.48 (s, 1H), 7.97-7.95 (m, 2H), 7.20-7.17 (m, 1H), 5.70 (bs, 2H), 3.87 (s, 3H), 3.82 (s, 3H). LC/MS (Method B): 225.1 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08202865B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-a4dfb99051f8486d833d4003466f4670 |
| 出典メモ | uspto-grants-2012_06 |