反应详情

温度

100 °C

[2-(2-Iodo-benzyl)-thiazolo[5,4-d]pyrimidin-7-yl]-(4-trifluoromethyl-phenyl)-amine (0.26, 0.50 mmol), palladium acetate (5.7 mg, 0.03 mmol), PPh3 (0.03 g, 0.10 mmol), and Cs2CO3 (0.21 g, 0.65 mmol) were combined in a sealed tube and placed under N2 atmosphere. Toluene (5 mL) was added followed by triisopropylsilanethiol (0.11, 0.55 mmol) and the resulting suspension was heated to 100° C. for 8 h. The reaction mixture was cooled to rt and filtered through a pad of diatomaceous earth. The filtrate was concentrated and purified by FCC to provide the title compound as a colorless solid (0.15 g, 60%). MS (ESI): mass calcd. for C28H33F3N4S2Si, 574.8; m/z found, 575.2 [M+H]+. 1H NMR (CDCl3): 8.65-8.60 (m, 1H), 8.14 (s, 1H), 7.99 (d, J=8.5 Hz, 2H), 7.65 (d, J=8.6 Hz, 2H), 7.57-7.53 (m, 1H), 7.35-7.32 (m, 1H), 7.25-7.18 (m, 2H), 4.79 (s, 2H)

1. temperatureThe reaction mixture was cooled to rt
2. filtrationfiltered through a pad of diatomaceous earth
3. concentrationThe filtrate was concentrated
4. custompurified by FCC