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 | Toluene | HCID 1140 | — |
| 生成物 | 4-[[4-(2-Methoxyphenyl)piperazin-1-yl]methyl]phenol | HCID 1377149 | 80% |
反応手順
One mole of 4-hydroxyphenyl methanol (124 g) and 192 g (2 moles) of 1-(2-methoxyphenyl)piperazine were dissolved in 1.5 liters of toluene. One mole (87 g) of lithium bromide and 0.1 mole (5.6 g) of potassium hydroxide were added portionwise, under stirring, and the reaction medium was heated to reflux for 5 hours. The reaction mixture was then allowed to cool to room temperature, and extracted twice with 500 ml of a 1N sodium hydroxide. The basic aqueous liquor was washed with 300 ml of toluene and then acidified to pH 7 with acetic acid to provoke precipitation of the desired product. The precipitate thus obtained was filtered off and then recrystallized from isopropanol, giving 238.4 g (0.80 mole, 80% yield) of the title product, 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-2542dc2b32b146868b33d1740dd7134d |
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| 出典メモ | uspto-grants-1992_08 |
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