反应详情

A mixture of 5-(4-fluoro-phenoxy)-isoindole-1,3-dione (42.9 g, 167 mmol), Bromo-acetic acid methyl ester (21.1 ml, 223 mmol), K2CO3 (62.3 g, 446 mmol) and Et2CO (700 ml) was refluxed with stirring for 16 h before the mixture was concentrated in vacuo. To the residue was added water (150 ml) and the resulting slurry was extracted with EtOAc (1×750 ml, 1×250 ml). The combined organic phases were dried over MgSO4 and concentrated in vacuo to give the title compound as a tan solid (49.7 g); 1H NMR (CDCl3) δ=7.80 (d, 1H), 7.01 to 7.30 (m, 6H), 4.41 (s, 2H), 3.76 (s, 3H).

1. temperaturewas refluxed
2. concentrationwas concentrated in vacuo
3. additionTo the residue was added water (150 ml)
4. extractionthe resulting slurry was extracted with EtOAc (1×750 ml, 1×250 ml)
5. dry with materialThe combined organic phases were dried over MgSO4
6. concentrationconcentrated in vacuo