反应详情

温度

65 °C

To a mixture of 5-Bromo-2-chloromethyl-pyridine hydrochloride (63.7 g, 0.262 mol) and N-hydroxylphthalimide (64 g, 0.393 mol) in acetonitrile (400 mL) was placed in water bath and added N,N-diisopropylethylamine (182 mL, 1.05 mol) using dropping funnel for 10 min. It was heated at 65° C. for 4 hrs and evaporated off the solvent and extra base. Then, water (100 mL) was added to the reaction mixture and stirred for overnight. The resulting solid was filtered, washed with water (2×50 mL) and acetonitrile (100 mL). The white solid was dried on vacuum pump to provide the title compound (84.2 g, 84%) as a white solid. MS-ESI m/z 334.95 (M+H)+.

1. customfor 10 min
2. customevaporated off the solvent and extra base
3. additionThen, water (100 mL) was added to the reaction mixture
4. filtrationThe resulting solid was filtered
5. washwashed with water (2×50 mL) and acetonitrile (100 mL)
6. customThe white solid was dried on vacuum pump