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Ammonium Acetate → 4,5,6,7-Tetrahydro-1-benzofuran-4-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | 4,5,6,7-Tetrahydro-1-benzofuran-4-one | HCID 2733541 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4,5,6,7-Tetrahydro-1-benzofuran-4-amine | HCID 18525171 | 38% |
反応手順
To a solution of 6,7-dihydro-1-benzofuran-4(5H)-one (2.0 g) in methanol (50 ml) was added 3 Å sieves (15 g), ammonium acetate (11.3 g) and sodium cyanoborohydride (1.22 g). After 48 h of stirring, the reaction mixture was filtered through celite, concentrated, dissolved in 1 N HCl (100 ml) and washed with ethyl ether (3×100 ml). The Aqueous layer was basified to pH 10 (NaOH), extracted methylene chloride (3×100 ml), dried MgSO4, filtered and concentrated to yield (760 mg, 38%) of the title compound as an oil:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06992087B2 |
| 出典データセット | uspto-grants-2006_01 |
| ORD ID | ord-3f6bba7a59fd4951a184dd8095483adf |
| 出典メモ | uspto-grants-2006_01 |