HRID1654782
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 5-nitro-6-bromo-1-indanone (11.0 g, 43 mmol) and bis(trimethylsilyloxy)ethane (22.0 mL, 90 mmol) in CH2Cl2 (90 mL) at room temperature was added trimethylsilyltrifluoromethanesulfonate (100 μL). The mixture was stirred for 2 h and the homogeneous solution was quenched with saturated aqueous NaHCO3 (100 mL). The CH2Cl2 layer was separated, washed with brine, dried over anhydrous MgSO4 and concentrated in vacuo. Chromatography over silica gel, eluting with ethyl acetate:hexanes (2:5), furnished 10.2 g (79%) of the title compound as a pale yellow solid.
WORKUP
后处理
- customthe homogeneous solution was quenched with saturated aqueous NaHCO3 (100 mL)
- customThe CH2Cl2 layer was separated
- washwashed with brine
- dry with materialdried over anhydrous MgSO4
- concentrationconcentrated in vacuo
- washChromatography over silica gel, eluting with ethyl acetate:hexanes (2:5)