反应详情

A solution of PhMgBr (prepared from 1.65 g of Mg (0.0678 mol) and 10.64 g of PhBr (0.0678 mol) in 40 mL of diethyl ether) was added to a mixture of 10 g (0.0565 mol) of 4-bromo-2-methylthiophene and 0.62 g (0.0012 mol) of NiCl2dppp in 50 mL of ether under stirring at reflux. The reaction mixture was refluxed for additional 3 h and then stirred overnight. The resulting mixture was treated with 10% aqueous NH4Cl, the organic layer was separated, washed with 10% aqueous NH4Cl and then dried with anhydrous Na2SO4. Solvent was evaporated, the residue was recrystallized from methanol. Yield 6.8 g (70%) of colorless crystals.

1. temperatureat reflux
2. temperatureThe reaction mixture was refluxed for additional 3 h
3. stirringstirred overnight
4. customthe organic layer was separated
5. washwashed with 10% aqueous NH4Cl
6. dry with materialdried with anhydrous Na2SO4
7. customSolvent was evaporated
8. customthe residue was recrystallized from methanol