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Aluminium lithium hydride → (4-(2-(Pyrrolidin-1-yl)ethoxy)phenyl)methanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | 4-[2-(1-Pyrrolidinyl)ethoxy]benzamide | HCID 22137456 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (4-(2-(Pyrrolidin-1-yl)ethoxy)phenyl)methanamine | HCID 14425929 | 101.7% |
反応手順
Lithium aluminum hydride (132 mg, 3.49 mmol, 2.1 eq.) was added to a solution of 4-[2-(1-pyrrolidinyl)ethoxy]benzamide (389 mg, 1.66 mmol) in dry THF (25 mL) then the reaction heated at reflux for 20 h. The reaction was allowed to cool to ambient temperature then quenched with water (0.250 mL). Aqueous sodium hydroxide (0.250 mL of 15% w/v) then water (0.750 mL) was added and the reaction stirred for 30 min. The reaction mixture was passed through a pad of diatomaceous earth which was washed with THF (3×15 mL). The combined organics were concentrated under reduced pressure to give the amine as oil (372 mg, >100%) which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06541499B1 |
| 出典データセット | uspto-grants-2003_04 |
| ORD ID | ord-b86e565b11d34e2b9e72f2191fa827f4 |
| 出典メモ | uspto-grants-2003_04 |