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1-Benzyl-(3R)-methylpiperazine-2-one → 1-Benzyl-3-methylpiperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Benzyl-(3R)-methylpiperazine-2-one | HCID 10013162 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Benzyl-3-methylpiperazine | HCID 2727520 | — |
反応手順
A mixture of 1-benzyl-3R-methylpiperazine-2-one (XX, 4.36 g), lithium aluminum hydride (LAH, 2.33 g) and THF (125 ml) is heated at reflux for 16 hr. After cooling to 20°-25°, the mixture is quenched slowly with water (2.3 ml), sodium hydroxide (10%, 3.5 ml) and water (5.7 ml). The residue is diluted with ether (100 ml) and is stirred for 1 hr. The solids are filtered and washed successively with ether, methylene chloride and ether. The combined filtrates are dried over potassium carbonate, filtered and concentrated to give 1-benzyl-(3R)-methylpiperazine (XXI), sufficiently pure to be carried on crude, NMR (CDCl3) 7.2-7.4, 3.49, 2.7-3.0, 1.95-2.1, 166, 1.3-1.7 and 1.01 δ.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05594140 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-2398a8523c694a7981b6f368416efd52 |
| 出典メモ | uspto-grants-1997_01 |