(Diethylamino)sulfur trifluoride → 1-Piperidineacetonitrile, 4-fluoro-
反応式
CCN(S(F)(F)[F:7])CC.O[CH:11]1[CH2:16][CH2:15][N:14]([CH2:17][C:18]#[N:19])[CH2:13][CH2:12]1>C(Cl)Cl>[F:7][CH:11]1[CH2:16][CH2:15][N:14]([CH2:17][C:18]#[N:19])[CH2:13][CH2:12]1参加物
4
実験手順
DAST (4.36 mL, 33 mmol) was added to a solution of (4-hydroxy-piperidin-1-yl)-acetonitrile (4.25 g, 30 mmol) in DCM (80 mL) at −30° C., the mixture was then stirred at rt for overnight. The reaction was cooled to −30° C. and quenched with methanol (10 mL) for 30 mins. The organic layer was then washed with NaHCO3 and dried. The residue was purified on a silica gel column to give 3 g (71%) of (4-fluoro-piperidin-1-yl)-acetonitrile.
後処理
- temperatureThe reaction was cooled to −30° C.
- customquenched with methanol (10 mL) for 30 mins
- washThe organic layer was then washed with NaHCO3
- customdried
- customThe residue was purified on a silica gel column
出典と根拠
- ORDレコード
- ord-40242723da6d462587b2a23680811fda
- 出典データセット
- uspto-grants-2003_07
- 特許番号
- US06599902B2
反応ノート
読み込み中…