反应详情

温度

80 °C

To a solution of methyl 3-(bromomethyl)-2-chlorobenzoate (748 mg, 2.84 mmol) in N,N-dimethylformamide (7 mL) was added sodium cyanate (412 mg, 8.41 mmol), and the mixture was stirred at 80° C. for 1 hr under nitrogen stream. The reaction mixture was diluted with a mixed solvent of ethyl acetate and hexane (1:1). The solution was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and filtrated. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane=2/98→20/80), and recrystallized from ethyl acetate and hexane to give the title compound (470 mg, 79%) as white crystals.

1. washThe solution was washed with water and saturated brine
2. dry with materialdried over anhydrous magnesium sulfate
3. filtrationfiltrated
4. customThe solvent was evaporated under reduced pressure
5. customthe obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane=2/98→20/80)
6. customrecrystallized from ethyl acetate and hexane