HRID1963318

反应详情

EQUATION

反应方程式

HRID 1963318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 2-(3,5-difluorobenzyl)isonicotinate (7.417 g, 28.18 mmol) was dissolved in acetic acid (72 mL) and platinum(IV) oxide (0.320 g, 1.41 mmol) was added. The mixture was hydrogenated in a Büchi hydrogenator at room temperature and 5 bar for 5 h. The reaction mixture was filtered through celite and the catalyst was washed with MeOH. The eluate was concentrated and DCM and 1 M K2CO3 were added. The phases were separated and the organic phase was washed with brine before it was dried and concentrated to yield methyl 2-(3,5-difluorobenzyl)piperidine-4-carboxylate (7.08 g, 93%). MS m/z 270 (M+H)+

WORKUP

后处理

  1. customwas hydrogenated in a Büchi hydrogenator at room temperature
  2. filtrationThe reaction mixture was filtered through celite
  3. washthe catalyst was washed with MeOH
  4. concentrationThe eluate was concentrated
  5. additionDCM and 1 M K2CO3 were added
  6. customThe phases were separated
  7. washthe organic phase was washed with brine before it
  8. customwas dried
  9. concentrationconcentrated