反应详情

温度

0 °C

Sodium hydride (1.11 g of 60% NaH in mineral oil) was added to a solution of CH3I (4.53 g) and N-(3-fluorophenyl)-3-iodobenzamide (7.26 g) in DMF (120 mL) at 0° C. under nitrogen. After being stirred at 0° C. for another 5 minutes, the reaction was stirred at room temperature under nitrogen for 4 h. The reaction was quenched by slow addition of saturated aqueous NH4Cl (120 mL), followed by addition of water (100 mL). The mixture was extracted with diethyl ether (300 mL×2). The combined ether layers were washed by water (150 mL×4) and brine (150 mL×1), dried by Na2SO4 and concentrated to give crude product (7.56 g), which was purified by column chromatography to afford N-(3-fluoro-phenyl)-3-iodo-N-methylbenzamide (5.88 g; 78%). 1H NMR (600 MHz, DMSO-d6) δ 7.64 (m, 2H), 7.28 (m, 1H), 7.24 (d, 1H, J=7.5 Hz), 7.19 (m, 1H), 7.04-6.99 (m, 3.33 (s, 3H).

1. stirringthe reaction was stirred at room temperature under nitrogen for 4 h
2. customThe reaction was quenched by slow addition of saturated aqueous NH4Cl (120 mL)
3. additionfollowed by addition of water (100 mL)
4. extractionThe mixture was extracted with diethyl ether (300 mL×2)
5. washThe combined ether layers were washed by water (150 mL×4) and brine (150 mL×1)
6. dry with materialdried by Na2SO4
7. concentrationconcentrated
8. customto give crude product (7.56 g), which
9. customwas purified by column chromatography