HRID1963318
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
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
- customwas hydrogenated in a Büchi hydrogenator at room temperature
- filtrationThe reaction mixture was filtered through celite
- washthe catalyst was washed with MeOH
- concentrationThe eluate was concentrated
- additionDCM and 1 M K2CO3 were added
- customThe phases were separated
- washthe organic phase was washed with brine before it
- customwas dried
- concentrationconcentrated