反应详情

温度

50 °C

To a stirred solution of dimethyl malonate (6.22 g, 47.1 mmol, 1.5 eq) in DMF (30 mL) was added K2CO3 (8.70 g, 63 mmol, 2.0 eq) and heated to 50° C. for 30 min when 1,2-difluoro-4-nitrobenzene (5.0 g, 31.4 mmol, 1.0 eq) was added and the reaction mixture was stirred for 5 h at 50° C. The reaction mixture was cooled to RT, filtered to remove K2CO3, and the DMF was evaporated under vacuum. The residue was diluted with EtOAc (100 mL), washed with water, brine, dried over Na2SO4 and evaporated to get dimethyl 2-(2-fluoro-4-nitrophenyl)malonate (6.5 g, 76%) as a solid (TLC system: EtOAc/PE (3:7), Rf: 0.50).

1. additionwas added
2. temperatureThe reaction mixture was cooled to RT
3. filtrationfiltered
4. customto remove K2CO3
5. customthe DMF was evaporated under vacuum
6. additionThe residue was diluted with EtOAc (100 mL)
7. washwashed with water, brine
8. dry with materialdried over Na2SO4
9. customevaporated