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Toluene → 1-Benzyl-4-hydroxy-4-(1,4-benzodioxan-5-yl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 1-Benzyl-4-piperidone | HCID 19220 | — |
| 反応物 | 5-Bromo-2,3-dihydro-1,4-benzodioxine | HCID 18787268 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Benzyl-4-hydroxy-4-(1,4-benzodioxan-5-yl)piperidine | HCID 19082002 | — |
反応手順
A toluene solution (10 ml) of 5-bromo-2,3-dihydrobenzo[1,4]dioxin (10 mmol) was stirred under argon at 0° C. and was treated with the dropwise addition of n-butyllithium (10 mmol) over ten minutes. After stirring for a further twenty minutes a solution of 1-benzyl-4-piperidone in toluene (10 mmol in 10 ml) was added dropwise over five minutes. Stirring was continued for two hours, at which point water (100 ml) was added and the product extracted into ethyl acetate (4×50 ml). The combined organics were washed with water (2×50 ml), brine (75 ml) and dried (MgSO4). Filtration and concentration in vacuo gave an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05763460 |
| 出典データセット | uspto-grants-1998_06 |
| ORD ID | ord-3739f71d30514f818eec72796ec5874e |
| 出典メモ | uspto-grants-1998_06 |