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
To a stirred solution of 5-[4-(benzyloxy)biphenyl-3-yl]-1-methyl-1H-pyrazole (Preparation 27, 3.0 g, 8.8 mmol) in methanol (26 mL) was added palladium on carbon (300 mg). The mixture was stirred under hydrogen gas for 16 hours. The reaction mixture was filtered through Celite™, and washed with tetrahydrofuran. The resulting filtrate was concentrated in vacuo. The residue was dissolved in ethyl acetate (26 mL) and degassed with argon prior to addition of palladium on carbon (300 mg). The reaction mixture was stirred under hydrogen gas for 6 hours. The reaction mixture was filtered through Celite™ and the filtrate concentrated in vacuo to give a solid. The solid was triturated with hexane to afford the title compound as a white solid (1.7 g, 77%).
WORKUP
后处理
- filtrationThe reaction mixture was filtered through Celite™
- washwashed with tetrahydrofuran
- concentrationThe resulting filtrate was concentrated in vacuo
- dissolutionThe residue was dissolved in ethyl acetate (26 mL)
- customdegassed with argon
- additionto addition of palladium on carbon (300 mg)
- stirringThe reaction mixture was stirred under hydrogen gas for 6 hours
- filtrationThe reaction mixture was filtered through Celite™
- concentrationthe filtrate concentrated in vacuo
- customto give a solid
- customThe solid was triturated with hexane