反应详情

温度

100 °C

1.07 g of 5-bromo-1-(2,6-dichlorophenyl)-3-(4-methoxybenzyl)-7-nitro-3,4-dihydroquinazolin-2(1H)-one (1.99 mmol) were dissolved in 26 mL of toluene. Na2CO3 (1.26 g, 11.9 mmol), 2-chlorophenylboronic acid (934 mg, 5.97 mmol), and ethanol/water (6.4 mL:6.4 mL) were added under argon followed by Pd(Ph3P)4 (115 mg, 0.0995 mmol). The resulting reaction mixture was stirred at 100° C. for ca.4 h, cooled to rt, diluted with 150 mL of ethyl acetate, washed with 2×100 mL of saturated aqueous NaHCO3 and 100 mL of brine, dried over Na2SO4, and concentrated under reduced pressure. The product was purified by flash chromatography on Biotage 40M column, eluting with 80:20 hexanes-acetone to yield 5-(2-chlorophenyl)-1-(2,6-dichlorophenyl)-3-(4-methoxybenzyl)-7-nitro-3,4-dihydroquinazolin-2(1H)-one. Mass spectrum (ESI) 568.1 (M+1).

1. customThe resulting reaction mixture
2. temperature4 h, cooled to rt
3. washwashed with 2×100 mL of saturated aqueous NaHCO3 and 100 mL of brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure
6. customThe product was purified by flash chromatography on Biotage 40M column
7. washeluting with 80:20 hexanes-acetone