HRID1708129
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 10 g (0.044 mol) of 7-bromo-1,2,3,4-tetrahydronaphthalenone in 300 mL of N-methylpyrrolidone was added 32.23 g (0.17 mol) of CuI and 31.59 g (0.17 mol) of sodium pentafluoropropanoate and the mixture was heated for 3 h at reflux under an argon atmosphere. After cooling to room temperature, the resulting suspension was poured into a mixture of H2O--Et2O (1:1) and filtered over celite. The layers were separated and the organic phase was washed with H2O and dried over MgSO4. The solvent was removed, to afford a residue that was chromatographed on silica gel (hexane-AcOEt), to give the desired product as a colourless oil (8.75 g, yield: 80%).
WORKUP
后处理
- temperaturethe mixture was heated for 3 h
- temperatureat reflux under an argon atmosphere
- additionthe resulting suspension was poured into a mixture of H2O--Et2O (1:1)
- filtrationfiltered over celite
- customThe layers were separated
- washthe organic phase was washed with H2O
- dry with materialdried over MgSO4
- customThe solvent was removed
- customto afford a residue that
- customwas chromatographed on silica gel (hexane-AcOEt)