HRID1026824
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 solution of the 347 (426 mg, 0.698 mmol) in DCM (10 ml) was added HCl in dioxane (0.7 ml, 4.01 eq, 2.80 mmol, 4M in dioxane) and the reaction mixture was stirred at RT for 3 hours. The mixture wad diluted with water and solid NaHCO3 was added. The reaction mixture was extracted well with EtOAc then the organic phase was collected, dried over Na2SO4, filtered and concentrated. The residue was purified by column chromatography (eluent 25% MeOH in EtOAc to 50% MeOH in EtOAc) to afford the desired compound 348 as a yellow powder (211 mg, 59% yield). MS (m/z)=511.4 (M+H).
WORKUP
后处理
- additionwas added
- extractionThe reaction mixture was extracted well with EtOAc
- customthe organic phase was collected
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by column chromatography (eluent 25% MeOH in EtOAc to 50% MeOH in EtOAc)