1-Aminopiperidine → 4-Chloro-N-1-piperidinylbutanamide
反応式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5](Cl)=[O:6].[N:8]1([NH2:14])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.C(=O)(O)[O-].[Na+]>ClCCl>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([NH:14][N:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1)=[O:6]参加物
5
実験手順
Add 4-chloro-butyryl chloride (5 mL, 43 mmol) to piperidin-1-ylamine (4.3 g, 43 mmol) in dichloromethane (100 mL) at room temp. Stir the reaction mixture at room temp for two hours. Add the reaction mixture into ice and saturated sodium bicarbonate solution. Extract the mixture with dichloromethane (100 mL). Wash the organic layer with saturated sodium bicarbonate solution (50 mL), dry with magnesium sulfate, filter and evaporate solvent under reduced pressure to obtain 5 g (57%) of the title compound as a white solid: Mass spectrum (ion spray): m/z=205.1 (M+H).
後処理
- extractionExtract the mixture with dichloromethane (100 mL)
- washWash the organic layer with saturated sodium bicarbonate solution (50 mL)
- dry with materialdry with magnesium sulfate
- filtrationfilter
- customevaporate solvent under reduced pressure
出典と根拠
- ORDレコード
- ord-a7233f75117c4518a69bc3d835a91033
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07713979B2
反応ノート
読み込み中…