Acetyl chloride → 1-(3-Hydroxypiperidin-1-yl)ethan-1-one
反応式
[OH:1][CH:2]1[CH2:7][CH2:6][CH2:5][NH:4][CH2:3]1.C(N(CC)CC)C.[C:15](Cl)(=[O:17])[CH3:16]>C1COCC1.C(Cl)Cl>[OH:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]([C:15](=[O:17])[CH3:16])[CH2:3]1参加物
6
反応条件
- 温度
- -78 °C
実験手順
3-Hydroxypiperidine (3.0 g, 30.0 mmol) was dissolved in THF (40 mL) and methylene chloride (40 mL). Triethylamine (7.47 g, 74.0 mmol) was added. The mixture was cooled to −78° C. and acetyl chloride (2.35 g, 30.0 mmol) was added drop wise. The mixture was warmed to r.t. and stirred under nitrogen for 1 about an hour. The solvents were removed under reduced pressure, and the resulting oil was purified using silica chromatography (2% methanol in ethyl acetate) to afford the title compound (3.57 g, 83%) as an oil.
後処理
- temperatureThe mixture was warmed to r.t.
- customThe solvents were removed under reduced pressure
- customthe resulting oil was purified
出典と根拠
- ORDレコード
- ord-ee7f708a522c4e49b678cf3f9f315113
- 出典データセット
- uspto-grants-2007_03
- 特許番号
- US07186715B2
反応ノート
読み込み中…