HRID595914
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a steel bomb, a solution of 6-fluoro-1′-methyl-[3,4′-bipyridin]-2′(1′H)-one (340 mg, 1.665 mmol) in MeOH (remaining 60% head space) was added followed by addition of Pd—C (Degussa) (354 mg, 0.333 mmol). After degassing with nitrogen stream, the steel bomb was filled with hydrogen (250 psi). The reaction mixture was stirred overnight. The reaction mixture was filtered off through Celite (washed with EtOAc/MeOH). The volatile materials were concentrated in vacuo to give crude (+/−)-4-(6-fluoropyridin-3-yl)-1-methylpiperidin-2-one (341 mg, 1.638 mmol, 98% yield) which was used for the next step without further purification. LCMS (m/z): 209.1 (MH+), 0.47 min.
WORKUP
后处理
- customAfter degassing with nitrogen stream
- additionthe steel bomb was filled with hydrogen (250 psi)
- filtrationThe reaction mixture was filtered off through Celite (washed with EtOAc/MeOH)
- concentrationThe volatile materials were concentrated in vacuo