HRID595914

反应详情

EQUATION

反应方程式

HRID 595914 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customAfter degassing with nitrogen stream
  2. additionthe steel bomb was filled with hydrogen (250 psi)
  3. filtrationThe reaction mixture was filtered off through Celite (washed with EtOAc/MeOH)
  4. concentrationThe volatile materials were concentrated in vacuo