反应详情

温度

120 °C

A mixture of 6-bromo-1H-indole (2.82 g, 14.41 mmol) and (E)-benzyl 2-methyl-3-(2-nitrovinyl)phenylcarbamate (3.0 g, 9.61 mmol) was dissolved in THF (50 mL) and NMP (0.5 mL). The THF was removed under vacuum, and the residue was heated at 120° C. for 16 hr and then at 125° C. for 6 hr. Upon cooling to room temperature, the mixture was dissolved in THF (50 mL). The resulting solution was diluted with ethyl acetate (250 mL), washed with water (3×80 mL) and brine (60 mL), and dried over anhydrous MgSO4. The desired product (3.00 g, 5.90 mmol, 61.4% yield) was isolated as a beige solid by ISCO (300 g silica gel, 25-60 ethyl acetate/hexane).

1. customThe THF was removed under vacuum
2. temperatureUpon cooling to room temperature
3. dissolutionthe mixture was dissolved in THF (50 mL)
4. additionThe resulting solution was diluted with ethyl acetate (250 mL)
5. washwashed with water (3×80 mL) and brine (60 mL)
6. dry with materialdried over anhydrous MgSO4