反应详情

A solution of 16.6 g (120 mmol) of K2CO3 in 50 ml of water is added to a solution of 15 g (50 mmol) of 4-bromo-2-fluoro-1-iodobenzene, 14.9 g (50 mmol) of 6 and 2.31 g (2 mmol) of [Pd(PPh3)4] in 100 ml of dioxane, and the mixture is refluxed overnight. The organic phase is washed with water and sat. NaCl, dried over MgSO4 and filtered through SiO2. The solvent is removed under reduced pressure, petroleum ether is added to the oily residue, and the product is recrystallised at −25° C. (yield: 88%, m.p. 78.0° C.).

1. temperaturethe mixture is refluxed overnight
2. washThe organic phase is washed with water and sat. NaCl
3. dry with materialdried over MgSO4
4. filtrationfiltered through SiO2
5. customThe solvent is removed under reduced pressure, petroleum ether
6. additionis added to the oily residue
7. customthe product is recrystallised at −25° C. (yield: 88%, m.p. 78.0° C.)