HRID720870
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
Compound 38 (0.52 g, 1.1 mmol) and compound 12 (0.55 g, 1.1 mmol) were dissolved in DMF and HBTU (0.8 g, 2.1 mmol) was added as a solid followed by DIEA (0.52 ml, 3 mmol). The reaction mixture was stirred at room temperature overnight, diluted with EtOAc and the organic phase washed with saturated NaHCO3, brine, dried over MgSO4, filtered and concentrated to an oil. This oil was purified by flash silica chromatography (1 to 2 to 3 to 4 to 5% MeOH/CH2Cl2) to give a yellow foam (0.45 g, 0.47 mmol, 43%, compound 39).
WORKUP
后处理
- washthe organic phase washed with saturated NaHCO3, brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated to an oil
- customThis oil was purified by flash silica chromatography (1 to 2 to 3 to 4 to 5% MeOH/CH2Cl2)