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Methanol → 7-Amino-2,3-dihydro-1,5-benzoxazepin-4(5H)-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-2,3-dihydro-1,5-benzoxazepin-4(5H)-one | HCID 57415944 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 生成物 | 7-Amino-2,3-dihydro-1,5-benzoxazepin-4(5H)-one | HCID 57853833 | 70% |
反応手順
Into a Hydrogenation flask containing 2-Nitro-6,7-dihydro-9H-5-oxa-9-aza-benzocyclohepten-8-one (0.2 g, 0.001 mol), was added Methanol (20 mL, 0.5 mol), followed by 10% Pd/C (0.02 g). The reaction mixture was shaken in a Parr apparatus under 20 psi of H2 for 90 min, was filtered through celite, washed with MeOH, and concentrated under reduced pressure to obtain 114 mg (70% yield) of title compound as a pale yellow solid. 97% purity, MP=158-160. LCMS: 179.19 (M+1), NMR (CDCl3) δ 7.94 (bs, 1H), 6.87 (d, J=8.4 Hz, 1H), 6.40 (dd, J=2.2 Hz, 8.5 Hz, 1H), 6.28 (s, 1H), 4.43-4.40 (m, 2H), 3.58 (bs, 2H), 2.79-2.76 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08148391B2 |
| 出典データセット | uspto-grants-2012_04 |
| ORD ID | ord-926b1c77f43b4b19a246a5195e35c7f5 |
| 出典メモ | uspto-grants-2012_04 |