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
A 250 flask charged with benzyl 4-(difluoromethyl)piperidine-1-carboxylate (1.16 g, 4.31 mmol), palladium, 10 wt. % (dry basis) on activated carbon, wet, degussa type e101 ne/w (0.563 g, 0.265 mmol) and EtOH (25 mL) was evacuated/backfilled with hydrogen (1 atm, 3×). After stirring overnight at room temperature, more palladium, 10 wt. % (dry basis) on activated carbon, wet, degussa type e101 ne/w (1.09 g) was added and the reaction was evacuated/backfilled with hydrogen (1 atm, 3×). After stirring overnight the reaction was filtered through a pad of Celite and the pad was washed with EtOH. Concentration of the filtrate in vacuo gave 4-(difluoromethyl)piperidine as a light-yellow oil (90 mg, 15% yield).
WORKUP
后处理
- dry with materialmore palladium, 10 wt. % (dry basis) on activated carbon
- additionwet, degussa type e101 ne/w (1.09 g) was added
- stirringAfter stirring overnight the reaction
- filtrationwas filtered through a pad of Celite
- washthe pad was washed with EtOH