反应详情

温度

170 °C

A mixture of N-{4-bromo-2-nitro-6-[(phenylmethyl)oxy]phenyl}acetamide (6.5 g, 17.8 mmol, STEP 1), zinc cyanide (4.18 g, 35.6 mmol), and tetrakis(triphenylphosphine)palladium (2.06 g, 1.78 mmol) in N,N-dimethylformamide (100 mL) was heated to 170° C. for 20 minutes in the microwave synthesizer (Biotage, Emrys Optimizer). After cooling to room temperature, the suspension was filtered, and washed with ethyl acetate. The organic layers were combined, washed with water, dried over magnesium sulfate, and concentrated in vacuum. The residual solid was purified by column chromatography on silica gel eluting with hexane/ethyl acetate (3:1) to afford the title compound as a white solid (5.5 g, 99%).

1. temperatureAfter cooling to room temperature
2. filtrationthe suspension was filtered
3. washwashed with ethyl acetate
4. washwashed with water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuum
7. customThe residual solid was purified by column chromatography on silica gel eluting with hexane/ethyl acetate (3:1)