HRID8810
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 25 mL rb flask equipped with a magnetic stir bar was added 0.309 g(0.86 mmol) of the product of Step A, 0.422 g (1.29 mmol) of cesium carbonate, 3 mL DMF and finally 145 μL of 1-bromopinacolone was added. The reaction mixture was stirred at room temperature for 1.5 h then partitioned between EtOAc and water. The organic layer was separated, washed with 10% aq. NaHSO4, water, brine, dried (MgSO4), filtered and evaporated. The residue was purified on s silica gel flash chromatography column eluted with 0–10% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound.
WORKUP
后处理
- customTo a 25 mL rb flask equipped with a magnetic stir bar
- additionwas added
- customthen partitioned between EtOAc and water
- customThe organic layer was separated
- washwashed with 10% aq. NaHSO4, water, brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated
- customThe residue was purified on s silica gel flash chromatography column
- washeluted with 0–10% EtOAc-hexane
- customEvaporation of the purified fractions
- customdrying in vacuo