反应详情

温度

80 °C

Sodium hydroxide (4.49 g, 112.3 mmol) was added at room temperature to a stirred solution of 1-chloro-2-fluoro-4-methoxy-5-nitrobenzene (11.0 g, 53.5 mmol) and dimethyl malonate (8.976 g, 67.9 mmol) in N-methylpyrrolidinone (110 mL). The mixture was heated to 80° C. for 2 hours then cooled to 5° C. The pH of the mixture was adjusted to 2 using aq. 1N HCl solution then water (600 mL) was added gradually with stirring over 15 minute at 5° C. The precipitated solid was collected by filtration and washed with water (2×20 mL). The filtered solid was dissolved in dichloromethane (150 mL), dried (Na2SO4) and concentrated under reduced pressure to give the title compound (15.5 g, 91%).

1. temperaturethen cooled to 5° C
2. filtrationThe precipitated solid was collected by filtration
3. washwashed with water (2×20 mL)
4. dissolutionThe filtered solid was dissolved in dichloromethane (150 mL)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated under reduced pressure