HRID1963267

反应详情

EQUATION

反应方程式

HRID 1963267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 2-(4-fluorobenzyl)isonicotinate (5.06 g, 20.63 mmol) was dissolved in acetic acid (50 mL) and platinum(IV) oxide (0.234 g, 1.03 mmol) added. The resulting mixture was hydrogenated in a Büchi hydrogenator overnight at room temperature and 5 bar. The catalyst was filtered off and washed with MeOH and the eluate evaporated. DCM and 10% K2CO3 were added and the phases separated. The aqueous phase was extracted with DCM and the combined organic phase washed with brine, passed through a phase separator and evaporated to yield methyl 2-(4-fluorobenzyl)piperidine-4-carboxylate (3.816 g, 73.6%) as a yellow oil. MS m/z 252 (M+H)+

WORKUP

后处理

  1. customwas hydrogenated in a Büchi hydrogenator overnight at room temperature
  2. filtrationThe catalyst was filtered off
  3. washwashed with MeOH
  4. additionDCM and 10% K2CO3 were added
  5. customthe phases separated
  6. extractionThe aqueous phase was extracted with DCM
  7. washthe combined organic phase washed with brine
  8. customevaporated