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Aluminium lithium hydride → 1-[2-(2-Fluorophenoxy)-ethyl]-4-[3-(3,4,5-trimethoxyphenyl)propyl]-piperazine dihydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | 1-{4-[2-(2-Fluorophenoxy)ethyl]piperazin-1-yl}-3-(3,4,5-trimethoxyphenyl)propan-1-one hydrochloride | HCID 67298802 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-[2-(2-Fluorophenoxy)-ethyl]-4-[3-(3,4,5-trimethoxyphenyl)propyl]-piperazine dihydrochloride | HCID 67299219 | 173.7% |
反応手順
To a solution of 1-{4-[2-(2-fluorophenoxy)ethyl]piperazin-1-yl}-3-(3,4,5-trimethoxyphenyl)-propan-1-one hydrochloride (0.2 g, 0.41 mmol) in THF (50 mL) was added LiAlH4 (0.2 g, 5 mmol). The reaction mixture was stirred under N2 for a day, cooled with an ice bath, and quenched with water (0.2 mL) and 10N NaOH aqueous solution (0.2 mL). The solid was filtered and the filtrate was concentrated to dryness. The residue was treated with ether and 2N HCl in ether (2 mL). The white solid was filtered and dried under vacuum to yield the title compound (0.18 g, 87%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08183374B2 |
| 出典データセット | uspto-grants-2012_05 |
| ORD ID | ord-51b4db710de04d45974849d18197797c |
| 出典メモ | uspto-grants-2012_05 |