HRID2206682
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 suspension of compound 26 (1.50 g, 1.82 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.22 g, 0.18 mmol) in THF (20 mL) was added NaBH4 (0.56 g, 14.6 mmol) at 0° C. The mixture was warmed up to r.t. slowly and stirred at r.t. for 12 hours. The reaction mixture was cooled to 0° C. and aqueous saturated NH4Cl solution (50 mL) was added to the mixture. The mixture was extracted with EtOAc (100 mL). The organic layer was washed with brine, dried over anhydrous MgSO4, filtered and concentrated in vacuo. The residue was purified using normal phase column chromatography to provide the title product 27 (0.98 g, 68%).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to 0° C.
- extractionThe mixture was extracted with EtOAc (100 mL)
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was purified