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Methanol → 7-amino-3,4-dihydro-2H-1,4-benzoxazin-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 7-nitro-3,4-dihydro-2H-1,4-benzoxazin-3-one | HCID 2763830 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 7-amino-3,4-dihydro-2H-1,4-benzoxazin-3-one | HCID 2764182 | 92.3% |
反応手順
7-Nitro-4H-benzo[1,4]oxazin-3-one (0.65 g, 3.3 mmol) and 10% palladium on carbon (0.13 g) were combined in EtOAc (15 mL) and MeOH (15 mL) and hydrogenated for 2 h at atmospheric pressure. The catalyst was removed by filtration through celite and the filtrate reduced in vacuo to yield the title compound as a colourless oil (0.50 g, 91%). δH (DMSO-d6) 4.42 (2H, s), 4.89 (2H, br s), 6.13-6.20 (2H, m), 6.56 (1H, d, J 8.1 Hz), 10.27 (1H, br s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08093238B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-dbf68fd6059442cc92254761fb481355 |
| 出典メモ | uspto-grants-2012_01 |