反应详情

To a solution of 2-(4-bromo-3-[1,3]dioxolan-2-yl-phenoxy)-6-[(2-hydroxy-ethyl)-methyl-amino]-nicotinonitrile (8) (400 mg, 0.95 mmol) in THF (30 mL) was added HCl solution (1 M, 10 mL). The reaction was stirred at room temperature overnight. After the reaction, all THF was evaporated under vacuum. The aqueous solution was extracted with EtOAc (2×50 mL). The organic layer was washed with water (3×50 mL). The organic layer was dried over MgSO4, filtered and evaporated under vacuum to afford the desired product 320 mg (89% yield) that was used without further purification. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 10.35 (s, 1 H), 7.91 (d, J=2.7 Hz, 1 H), 7.67 (t, J=9.2 Hz, 2 H), 7.32 (dd, J=8.6, 2.7 Hz, 1 H), 6.24 (d, J=8.6 Hz, 1 H), 3.70-3.62 (m, 2 H), 3.56-3.49 (m, 2 H), 3.04 (s, 3 H).

1. customAfter the reaction
2. customall THF was evaporated under vacuum
3. extractionThe aqueous solution was extracted with EtOAc (2×50 mL)
4. washThe organic layer was washed with water (3×50 mL)
5. dry with materialThe organic layer was dried over MgSO4
6. filtrationfiltered
7. customevaporated under vacuum