反应详情

温度

40 °C

A mixture of the product of Example 34, Step A (0.087 g; 0.5 mmol), 6-propylnicotinic acid (0.082 g; 0.5 mmol) and EDC (0.11 g; 0.57 mmol) in anhydrous DMSO (2 ml) was stirred for 1 h at ˜40° C. under N2. To this 1M TBAF in THF (0.5 ml) was added and the resulting mixture was stirred for 1 h at ˜110° C. After cooling to room temperature the mixture was diluted to 15 ml with EtOAc, washed with H2O, brine, dried over anhydrous MgSO4, filtered and filtrate evaporated to dryness. The residue was purified by FCC (SiO2, CH2Cl2:EtOAc 9:1) to give the title compound (0.05 g; 33%), as colorless solid. 1H-NMR (CDCl3) 1.0 (m, 3H); 1.8 (m, 2H); 2.88 (tr, 2H, J=9 Hz); 7.3-7.4 (m, 4H); 7.57 (d, 1H, J=9 Hz); 8.08 (dd, 1H, J=2, 9 Hz); 8.38-8.43 (m, 2H); 9.39 (d, 1H, J=2 Hz).

1. stirringthe resulting mixture was stirred for 1 h at ˜110° C
2. temperatureAfter cooling to room temperature the mixture
3. washwashed with H2O, brine
4. dry with materialdried over anhydrous MgSO4
5. filtrationfiltered
6. customfiltrate evaporated to dryness
7. customThe residue was purified by FCC (SiO2, CH2Cl2:EtOAc 9:1)