反应详情

A mixture of (4-(diphenylamino)phenyl)boronic acid (1.5 g, 5.19 mmol), 4-iodo-1-bromobenzene (1.33 g, 4.71 mmol), Na2CO3 (1.78 g, 16.8 mmol) and Pd(PPh3)4 (0.163 g, 0.141 mmol) in THF/H2O (28 mL/17 mL) was degassed and the resulting mixture was heated at reflux overnight under an argon atmosphere. After cooling, the mixture was poured into dichloromethane (150 mL), then washed with water (2×150 mL) and brine (100 mL). The organic phase was dried over Na2SO4, purified with flash column chromatography (silica gel, hexanes/ethyl acetate 50:1) then recrystallized in dichloromethane/methanol to afford a white solid (Compound 35)(1.64 g, in 87% yield).

1. customwas degassed
2. temperaturethe resulting mixture was heated
3. temperatureat reflux overnight under an argon atmosphere
4. temperatureAfter cooling
5. additionthe mixture was poured into dichloromethane (150 mL)
6. washwashed with water (2×150 mL) and brine (100 mL)
7. dry with materialThe organic phase was dried over Na2SO4
8. custompurified with flash column chromatography (silica gel, hexanes/ethyl acetate 50:1)
9. customthen recrystallized in dichloromethane/methanol