化工社化工社 化学情報印刷レポート · 研究参考用
3-Bromo-1-propanol → 3-[(2R)-2-Methylpyrrolidin-1-yl]propan-1-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Bromo-1-propanol | HCID 12308 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | (R)-2-Methylpyrrolidine | HCID 641544 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ammonia | HCID 222 | — |
| 生成物 | 3-[(2R)-2-Methylpyrrolidin-1-yl]propan-1-ol | HCID 57457560 | 65% |
反応手順
3-Bromopropan-1-ol (5.28 mL, 58.4 mmol) was added to a solution of (R)-2-methylpyrrolidine (7.1 g, 58.4 mmol) in water (200 mL). KOH (7.53 g, 134 mmol) was then added and the mixture stirred at ambient temperature for 48 hours. The reaction mixture was then extracted with dichloromethane (5×80 mL) and ethyl acetate (5×80 mL). The combined organic extracts were dried using MgSO4, filtered and concentrated in vacuo. The compound was purified by column chromatography on Biotage® silica gel, eluting with dichloromethane:methanol:ammonia, (90:10:1) to give the title compound as a pale brown oil (5.44, 65%). LCMS (APCI+) 144 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07456164B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-7c1f6287be084aeea3f72847f4bb79fc |
| 出典メモ | uspto-grants-2008_11 |