反应详情

温度

80 °C

A 20 mL reaction vial equipped with a stir bar was charged with 4-fluoro-2-methoxy-1-nitrobenzene (0.5 g, 2.92 mmol), 1-amino-2-methylpropan-2-ol (0.313 g, 3.51 mmol), N-methyl-2-pyrrolidinone (7.3 mL) and Hunig's base (N,N-diisopropylethylamine) (0.76 g, 5.84 mmol). The vessel was sealed and the reaction was heated on a thermal block at 80° C. for 24 hours. The reaction was cooled to ambient temperature, treated with water (40 mL) and extracted with ethyl acetate (3×60 mL). The combined organic layers were washed with brine (25 mL), dried over Na2SO4, filtered, and concentrated. The concentrate was purified by flash chromatography on a 10 g silica gel column with 1% methanol/CH2Cl2 to provide the title compound.

1. customA 20 mL reaction
2. customvial equipped with a stir bar
3. customThe vessel was sealed
4. temperatureThe reaction was cooled to ambient temperature
5. extractionextracted with ethyl acetate (3×60 mL)
6. washThe combined organic layers were washed with brine (25 mL)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated
10. customThe concentrate was purified by flash chromatography on a 10 g silica gel column with 1% methanol/CH2Cl2