反应详情

温度

120 °C

A mixture of the product of Step A (0.31 g, 1.44 mmol), the product of Example 34, Step A (0.25 g, 1.44 mmol), EDC (0.36 g, 1.87 mmol) and HOBT (0.01 g) in anhydrous DMF (1 ml) was stirred overnight at 40° C. 1M solution of TBAF in THF (0.25 mL) was added to it and mixture was stirred for 3 h at 120° C. This was diluted to 20 ml with H2O and extracted with EtOAc (50 ml). The organic layer was separated, dried over MgSO4 and filtered. The filtrate was evaporated to dryness and the residue was purified by FCC (SiO2) and crystallized from MeOH to give the title compound (0.17 g; 33.3%) as creamy crystalline solid. 1H-NMR (CDCl3) 1.43 (d, 6H, J=6.06 Hz); 7.65-7.74 (m, 1H); 7.05 (d, 1H, J=8.76 Hz); 7.3-7.38 (m, 3H); 7.55 (d, 1H, J=8.14 Hz); 8.1-8.03 (m, 2H); 8.28 (d, 1H, J=2.13 Hz); 8.4 (broad s, 1H).

1. extractionextracted with EtOAc (50 ml)
2. customThe organic layer was separated
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customThe filtrate was evaporated to dryness
6. customthe residue was purified by FCC (SiO2)
7. customcrystallized from MeOH