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1-[1-(2-Chloro-4-nitrophenyl)piperidin-4-yl]-1,4-dihydro-2h-3,1-benzoxazin-2-one → 1-[1-(4-Amino-2-chlorophenyl)piperidin-4-yl]-1,4-dihydro-2H-3,1-benzoxazin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-[1-(2-Chloro-4-nitrophenyl)piperidin-4-yl]-1,4-dihydro-2h-3,1-benzoxazin-2-one | HCID 22644572 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-[1-(4-Amino-2-chlorophenyl)piperidin-4-yl]-1,4-dihydro-2H-3,1-benzoxazin-2-one | HCID 22644680 | — |
反応手順
Iron powder (1.5 g) was added to a solution of the product from step (i) (1.37 g) in acetic acid (50 ml) and tetrahydrofuran (20 ml). After stirring at room temperature for 5 h, the mixture was filtered through celite, the solvent removed under reduced pressure and the residue partitioned between ethyl acetate and aqueous sodium hydrogencarbonate solution. The organic layer was washed with water, dried and evaporated under reduced pressure. Purification was by chromatography eluting with 50% ethyl acetate/isohexane. Yield 1.05 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06812226B2 |
| 出典データセット | uspto-grants-2004_11 |
| ORD ID | ord-7ada653c34424853b26131f5dcd74ffb |
| 出典メモ | uspto-grants-2004_11 |