HRID1708129

反应详情

EQUATION

反应方程式

HRID 1708129 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturethe mixture was heated for 3 h
  2. temperatureat reflux under an argon atmosphere
  3. additionthe resulting suspension was poured into a mixture of H2O--Et2O (1:1)
  4. filtrationfiltered over celite
  5. customThe layers were separated
  6. washthe organic phase was washed with H2O
  7. dry with materialdried over MgSO4
  8. customThe solvent was removed
  9. customto afford a residue that
  10. customwas chromatographed on silica gel (hexane-AcOEt)