反应详情

To a stirred solution of 2-(4-(ethylsulfonyl)-2-methoxyphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (Preparation 21, 600 mg, 1.84 mmol) in dioxane (30 mL) and water (10 mL) were added 4-bromo-2-iodophenol (604 mg, 2.02 mmol), sodium carbonate (488 mg, 4.6 mmol) and tetrakis(triphenylphosphine)palladium(0) (106 mg, 0.092 mmol). The reaction was stirred at reflux for 18 hours. The reaction was allowed to cool temperature and then filtered through celite. The filtrate was reduced to dryness and then purified by silica gel column chromatography eluting with cyclohexane:EtOAc 1:1 followed by a second silica gel column chromatography eluting with CH2Cl2:MeOH 98:2 to give the title compound as pale yellow solid in 44% yield, 301 mg.

1. temperatureat reflux for 18 hours
2. temperatureto cool temperature
3. filtrationfiltered through celite
4. custompurified by silica gel column chromatography
5. washeluting with cyclohexane:EtOAc 1:1
6. washeluting with CH2Cl2:MeOH 98:2