反应详情

温度

80 °C

3-Chloro 4-fluoro nitrobenzene (5.0 g, 28.48 mmol) and dimethyl malonate (3.3 mL, 36.17 mmol) were dissolved in N-methylpyrrolidinone (131.5 mL). Sodium hydroxide (2.4 g, 60 mmol) was added at RT and the solution was heated at 80° C. for 2 hours. The reaction mixture was cooled to 5° C. and 1N HCl solution was added to give a pH of 2. Water (526 mL) was added and the resulting mixture was stirred for 15 minutes during which a pale yellow solid precipitated out. The precipitate was collected by filtration and then washed with water (2×10 mL). The resulting solid mass was dissolved in DCM (50 mL), dried (Na2SO4) and then the volatiles were removed under reduced pressure to afford the title compound (5.5 g, 67%). The product was used as such in the next step without purification.

1. temperatureThe reaction mixture was cooled to 5° C.
2. customto give a pH of 2
3. customprecipitated out
4. filtrationThe precipitate was collected by filtration
5. washwashed with water (2×10 mL)
6. dissolutionThe resulting solid mass was dissolved in DCM (50 mL)
7. dry with materialdried (Na2SO4)
8. customthe volatiles were removed under reduced pressure