関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-(4-Benzyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanone | HCID 10322760 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 10435214 | HCID 10435214 | 79% |
反応手順
In 24 ml of tetrahydrofuran was suspended 0.60 g (16 mmol) of lithium aluminum hydride, to which a suspension consisting of 24 ml of tetrahydrofuran and 3.0 g (6.3 mmol) of 1-(4-benzyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanone was added portionwise under ice-cooled conditions. After being stirred for 0.5 hour, the resultant mixture was added dropwise with 5 ml of ethyl acetate, followed by further addition of 50 ml of ethyl acetate. The thus prepared solution was poured into an aqueous solution of ammonium chloride, and the organic layer was separated. The organic layer was washed twice with saturated saline and then dried over anhydrous sodium sulfate. The solvent was removed, and the residue was recrystallized from a mixed solvent of ethanol and chloroform to give 2.37 g of 1-(4-benzyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanol (yield: 79%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04528194 |
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| 出典データセット | uspto-grants-1985_07 |
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| ORD ID | ord-63c838f4feed4e71ab42cffecb96d306 |
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| 出典メモ | uspto-grants-1985_07 |
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