反应详情

温度

125 °C

Using a method similar to Example 16 d), 3.61 g (0.020 mol) of (1), 3.0 g (0.022 mol) of 4-methylphenylboronic acid, 4.66 g (0.044 mol) of sodium carbonate were placed in 60 ml of ethylene glycol/12 ml of water in the reaction vessel, the mixture was degassed a number of times and saturated with argon. After addition of 22.4 mg (0.1 mmol) of palladium acetate and 0.114 g (0.2 mmol) of TMSPP, the reaction mixture was stirred for 2 hours at 125° C. After addition of 60 ml of water, the aqueous phase was extracted 4 times with 50 ml each time of ether, the combined ether phases were washed with 50 ml of water and 50 ml of saturated sodium chloride solution and dried over magnesium sulfate. Removal of the solvent gave 4.5 g of (21) as solid.

1. customsimilar to Example 16 d
2. customthe mixture was degassed a number of times
3. extractionthe aqueous phase was extracted 4 times with 50 ml each time of ether
4. washthe combined ether phases were washed with 50 ml of water and 50 ml of saturated sodium chloride solution
5. dry with materialdried over magnesium sulfate
6. customRemoval of the solvent