反应详情

To a stirred mixture of 4-((dimethylamino)methyl)benzaldehyde (4 g, 24.5 mmol) and anhydrous magnesium sulfate (15.8 g, 111.5 mmol) in anhydrous acetonitrile (100 mL) was added 4-amino-6-fluoroisobenzofuran-1(3H)-one (4 g, 22.3 mmol) at 0° C. After the addition, the mixture was stirred at reflux for 3 days. The mixture was filtered and the cake was washed with ethyl acetate (50 mL×3). The filtrate was concentrated to give crude product, which was re-crystallized with isopropanol to give the title compound (3.7 g, yield 55%). LC-MS (ESI) m/z: 314 (M+1)+.

1. additionAfter the addition
2. temperatureat reflux for 3 days
3. filtrationThe mixture was filtered
4. washthe cake was washed with ethyl acetate (50 mL×3)
5. concentrationThe filtrate was concentrated
6. customto give crude product, which
7. customwas re-crystallized with isopropanol