HRID45847
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
Dibenzyl-[3-(1-ethyl-4-pyridin-4-yl-1H-pyrazol-3-yl)-2,4-difluoro-phenyl]-amine (2.35 g, 4.89 mmol) was dissolved in methanol (140 mL). 20% Palladium hydroxide on carbon (500 mg) was added and the reaction was stirred under hydrogen atmosphere (50 psi) for 7 h. A further addition of catalyst was made (500 mg) and hydrogenation was continued for 6 more hours. The reaction mixture was filtered over a Celite pad and then concentrated under reduced pressure. The crude product was purified by flash chromatography on silica gel (DCM/methanol 95:5) to give 1.16 g of the desired product as a colourless foam (79% yield).
WORKUP
后处理
- additionA further addition of catalyst
- filtrationThe reaction mixture was filtered over a Celite pad
- concentrationconcentrated under reduced pressure
- customThe crude product was purified by flash chromatography on silica gel (DCM/methanol 95:5)