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2-Propylpiperidine → 4-(2-Propyl-piperidin-1-yl)-butyronitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Propylpiperidine | HCID 9985 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Bromobutyronitrile | HCID 21412 | — |
| 反応物 | Dichloromethane methanol | HCID 21226129 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 4-(2-Propyl-piperidin-1-yl)-butyronitrile | HCID 18626322 | 83% |
反応手順
A mixture of 2-propylpiperidine (550 mg, 4.3 mmol), 4-bromobutyronitrile (430 mg, 3.0 mmol) and potassium carbonate (550 mg, 4.0 mmol) in acetonitrile (5 mL) was stirred at rt for 12 h., followed by addition of a saturated brine (25 mL). The reaction mixture was extracted with ethyl acetate (3×25 mL) and the combined organic phases were dried (MgSO4) and evaporated to dryness to produce crude 8. The crude product was subjected to CC [eluent: CH2Cl2: MeOH (99: 1)] to give pure 8 (0.48 g, 83%); LC-MS [M+H]+194 (cald. 194.2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06528529B1 |
| 出典データセット | uspto-grants-2003_03 |
| ORD ID | ord-b0ad0b4a84f843378a0a9731812c0337 |
| 出典メモ | uspto-grants-2003_03 |