反应详情

To a stirred solution of dimethyl 2-(4-nitrophenyl)malonate (10 g, 39.52 mmol, 1.0 eq) and K2CO3 (10.9 g 79.05 mmol 2.0 eq) in DMF (40 mL), was added methyl iodide (4.94 mL, 79.05 mmol 2.0 eq) at 0° C. and the mixture stirred at RT for 18 h. K2CO3 was filtered out and the filtrate concentrated under vacuum. The residue was diluted with water (80 mL) and extracted with EtOAc (2×80 mL). The organic layer was separated washed with brine solution, dried over anhydrous Na2SO4 and the solvent evaporated to get dimethyl 2-methyl-2-(4-nitrophenyl)malonate (7 g, 66%; TLC system: EtOAc/PE (3:7), Rf: 0.5.)

1. filtrationK2CO3 was filtered out
2. concentrationthe filtrate concentrated under vacuum
3. additionThe residue was diluted with water (80 mL)
4. extractionextracted with EtOAc (2×80 mL)
5. customThe organic layer was separated
6. washwashed with brine solution
7. dry with materialdried over anhydrous Na2SO4
8. customthe solvent evaporated