反应详情

温度

-78 °C

To a solution of thiazole (5 eq) in dry THF, BuLi (5 eq) was added dropwise at −78° C. and this was stirred at −78° C. for 30 min. ZnCl2 (1M in ether, 5 eq) was added and stirred at 0° C. for 30 min, then Intermediate B (1 eq) and Pd(dppf)Cl2 (0.1 eq) were added. The reaction was heated to 70° C. for 16 h; then the mixture was diluted with EtOAc, washed with brine and concentrated. The residue was purified by silica gel flash chromatography to give the title compound. LCMS (0.05% TFA): 344.1 m/z (M+H)+; 1H-NMR (MeOD, 500 MHz): δ: 8.04 (bs, 1H), 7.99 (bs, 1H), 7.76 (bs, 1H), 4.41 (m, 2H), 3.42 (s, 3H), 2.16 (m, 2H), 2.09˜1.72 (m, 8H), 0.88 (t, 3H, J=7.5 Hz).

1. stirringstirred at 0° C. for 30 min
2. temperatureThe reaction was heated to 70° C. for 16 h
3. washwashed with brine
4. concentrationconcentrated
5. customThe residue was purified by silica gel flash chromatography