関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Hydroxybenzyl Alcohol | HCID 125 | — |
| 反応物 | 1-(2-Methoxyphenyl)piperazine | HCID 1346 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Lithium Bromide | HCID 82050 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-[[4-(2-Methoxyphenyl)piperazin-1-yl]methyl]phenol | HCID 1377149 | 56% |
反応手順
4-Hydroxyphenyl methanol (124 g, 1 mole) and 192 g (1 mole) of 1-(2-methoxyphenyl)piperazine, together with 56 g (1 mole) of potassium hydroxide and 8.7 g (0.1 mole) of lithium bromide and 32.2 g (0.1 mole) of Aliquat 366 were dissolved in a mixture of 1 liter of toluene and 1 liter of water. The reaction mixture was refluxed for 24 hours, and then allowed to cool to room temperature. The organic layer was decanted and extracted twice with 500 ml of a 10% sodium hydroxide solution. The basic aqueous liquor was treated with ammonium acetate to provoke precipitation of the desired product. After filtration and drying under vacuum overnight at 50° C., 167 g (0.56 mole, 56% yield) of the title product was obtained as small white leaflets melting at 172° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05142052 |
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| 出典データセット | uspto-grants-1992_08 |
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| ORD ID | ord-0ebeb5b64dfb451d93a06df6381c57ed |
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| 出典メモ | uspto-grants-1992_08 |
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