反应详情

温度

100 °C

To 250 mL flask was charged with 8-mercaptoadenine (2.00 g, 11.98 mmol), 5,6-dibromo-benzo-[1,3]dioxole (6.70 g, 24.0 mmol), Pd2dba3 (0.548 g, 0.599 mmol), Xantphos (0.693 g, 1.20 mmol), K2CO3 (3.31 g, 23.95 mmol), and dry dioxane (25 mL). The resulting mixture was heated at 100° C. for 16 h under nitrogen. After cooling, the reaction mixture was filtered and washed with a 2/2/0.5 mixture of CH2Cl2, EtOAc, and MeOH. The combined filtrates were concentrated in vacuo. The dark brown residue was purified by chromatography on SiO2 (CH2Cl2/EtOAc/MeOH, 2/2/0/5) and subsequent recrystallization from MeOH provided the title compound (1.4 g, 32%). 1H NMR (DMSO-d6) δ 8.08 (s, 1H), 7.38 (s, 1H), 7.23 (s, 1H), 6.12 (s, 2H).

1. temperatureAfter cooling
2. filtrationthe reaction mixture was filtered
3. washwashed with a 2/2/0.5 mixture of CH2Cl2, EtOAc, and MeOH
4. concentrationThe combined filtrates were concentrated in vacuo
5. customThe dark brown residue was purified by chromatography on SiO2 (CH2Cl2/EtOAc/MeOH, 2/2/0/5) and subsequent recrystallization from MeOH