反应详情

3M aq. NaOH (80 mL) was added to a solution of diethyl 2-(2,6-difluoro-4-methoxyphenyl)malonate, 6.30 g, 20.85 mmol) in Et2O (5 mL). The reaction mixture was heated at reflux until all the solid had dissolved. After cooling, the mixture was acidified with 3M aq. HCl and the product was extracted with EtOAc (2×100 ml). The combined organic layers were dried (MgSO4) and solvent was removed in vacuo to give the title compound as a tan coloured solid (4.50 g, 88%); mp 157° C. (dec); 1H NMR (270 MHz, DMSO-d6) 3.78 (3H, s, CH3), 4.72 (1H, s, CH), 6.70-6.79 (2H, m, ArH).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux until all the solid
3. dissolutionhad dissolved
4. temperatureAfter cooling
5. extractionthe product was extracted with EtOAc (2×100 ml)
6. dry with materialThe combined organic layers were dried (MgSO4) and solvent
7. customwas removed in vacuo