HRID1662714
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 2.10 g of the compound obtained in Step 139-1 in THF (100 ml) was added a solution 1 mol/L TBAF in THF (10 ml) under ice cooling and the reaction mixture was stirred at room temperature for two hours. Water was poured, the solution was extracted twice with CHCl3; the combined organic layer was washed with saturated brine and dried over MgSO4, then, the drying agent was separated by filtration and the solvent was evaporated under reduced pressure. The obtained residue was purified by column chromatography (silicagel 60N; mobile phase: CHCl3/MeOH=20/1 to 10/1; v/v) to obtain 1.79 g of the title compound.
WORKUP
后处理
- extractionthe solution was extracted twice with CHCl3
- washthe combined organic layer was washed with saturated brine
- dry with materialdried over MgSO4
- customthe drying agent was separated by filtration
- customthe solvent was evaporated under reduced pressure
- customThe obtained residue was purified by column chromatography (silicagel 60N; mobile phase: CHCl3/MeOH=20/1 to 10/1; v/v)