Sodium Carbonate → 1-(Cyclopropylmethyl)piperidin-4-one
反応式
Br[CH2:2][CH:3]1[CH2:5][CH2:4]1.Cl.O.[NH:8]1[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][CH2:9]1.C(=O)([O-])[O-].[Na+].[Na+]>C(#N)C>[CH:5]1([CH2:4][N:8]2[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][CH2:9]2)[CH2:3][CH2:2]1参加物
5
反応条件
- 温度
- 85 °C
実験手順
To a suspension of bromomethyl cyclopropane (4 mmol) and 4-piperidone hydrate hydrochloride (4 mmol) in acetonitrile (30 mL) was added sodium carbonate (11 mmol). The reaction mixture was stirred 16 h at 85° C. The resulting suspension was filtered and the solid was washed with acetonitrile. The filtrate was concentrated in vacuo and purified by column chromatography on silica eluting with DCM/2N NH3 in methanol 97:3 to yield 339 mg of the title compound as yellow oil. MS (m/e): 154.2 (MH+, 100%).
後処理
- filtrationThe resulting suspension was filtered
- washthe solid was washed with acetonitrile
- concentrationThe filtrate was concentrated in vacuo
- custompurified by column chromatography on silica eluting with DCM/2N NH3 in methanol 97:3
出典と根拠
- ORDレコード
- ord-6f8c09e36221499a9402e63f834e28db
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07456174B2
反応ノート
読み込み中…