反应详情

Under nitrogen, 3 g (2.6 mmol) of Pd(PPh3)4 was added to a stirred solution of 5.0 g (18 mmol) of 1,2-dibromo-4,5-difluorobenzene (Aldrich), 4.2 g (25 mmol) of 4-methylthiophenylboronic acid (Example 1, Step 2), and 3.1 g (22 mmol) of 4-fluorophenylboronic acid in 100 mL of toluene, 100 mL of ethanol, and 100 mL of 2M Na2CO3. After vigorous stirring at reflux overnight, the solvent was removed in vacuo and the residue dissolved in ethyl acetate. The resulting solution was washed with water and dried over MgSO4. Purification by silica gel chromatography gave 1,2-difluoro-4-(4-fluorophenyl)-5-[4-(methylthio)phenyl]benzene as a semi-solid which was used without further purification.

1. temperatureat reflux overnight
2. customthe solvent was removed in vacuo
3. dissolutionthe residue dissolved in ethyl acetate
4. washThe resulting solution was washed with water
5. dry with materialdried over MgSO4
6. customPurification by silica gel chromatography