HRID1963146

反应详情

EQUATION

反应方程式

HRID 1963146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 2-(4-(trifluoromethyl)phenyl)isonicotinate (4.985 g, 17.73 mmol) was dissolved in acetic acid (45 mL) and platinum(IV) oxide (0.232 g, 1.02 mmol) added. The resulting mixture was hydrogenated in a Büchi hydrogenator at room temperature and 5 bar for 5 h. More platinum(IV) oxide (0.116 g, 0.51 mmol) was added and the hydrogenation continued at 5 bar for 1 h. The catalyst was filtered off and washed with MeOH and the eluate evaporated. DCM and 10% K2CO3 were added and the phases separated. The organic layer was washed with brine, passed through a phase separator and evaporated to yield methyl 2-(4-(trifluoromethyl)phenyl)piperidine-4-carboxylate (5.04 g, 99%) as a brown oil. MS m/z 288 (M+H)+

WORKUP

后处理

  1. customwas hydrogenated in a Büchi hydrogenator at room temperature
  2. waitthe hydrogenation continued at 5 bar for 1 h
  3. filtrationThe catalyst was filtered off
  4. washwashed with MeOH
  5. additionDCM and 10% K2CO3 were added
  6. customthe phases separated
  7. washThe organic layer was washed with brine
  8. customevaporated