反応 #359739
ord-6f8c09e36221499a9402e63f834e28db
反応方程式
bromomethyl cyclopropane
4-piperidone hydrate hydrochloride
sodium carbonate
→
title compound
収率 55.3%
1-Cyclopropylmethyl-piperidin-4-one
収率 55.3%
反応条件
温度
85°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1ろ過The resulting suspension was filtered
- 2洗浄the solid was washed with acetonitrile
- 3濃縮The filtrate was concentrated in vacuo
- 4その他purified by column chromatography on silica eluting with DCM/2N NH3 in methanol 97:3
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%).