反应详情

温度

130 °C

To a suspension of 4 (0.12 g, 0.324 mmol), phthalic anhydride (0.060 g, 0.401 mmol), and sodium acetate (0.037 g, 0.434 mmol) was added acetic acid (1.5 mL) and the resulting mixture was stirred at 130° C. After 7 h, the mixture was quenched with sodium bicarbonate and extracted with DCM. The organic layer was dried over MgSO4 and concentrated. Purification by preparative HPLC afforded 12. Rf=0.32 (95:5 DCM:MeOH). 1H NMR (400 MHz, CDCl3) δ 8.05-7.64 (m, 5H), 7.44-7.27 (m, 4H), 5.16-5.00 (m, 2H), 4.90 (m, 1H), 3.34-3.09 (m, 3H), 2.92-2.77 (m, 1H), 2.77-2.45 (m, 3H), 2.36-2.18 (m, 1H), 2.17-1.99 (m, 1H), 1.38 (d, J=6.8 Hz, 2H). MS (ESI) m/z calcd for C25H26N3O6 [M+H]+ 464.5, found 464.3.

1. customthe mixture was quenched with sodium bicarbonate
2. extractionextracted with DCM
3. dry with materialThe organic layer was dried over MgSO4
4. concentrationconcentrated
5. customPurification by preparative HPLC