反应详情

温度

150 °C

111-1. A mixture of 9-iodo-3,4,7,8-tetrahydro-[1,4]diazepino[7,1-a]isoquinoline-2,5-dione (2.5 g, 7.06 mmol) in dioxane (15 mL) was treated with tributyl(1-ethoxyvinyl)stannane (2.98 mL, 8.82 mmol) and Pd(PPh3)4 (408 mg, 0.35 mmol) under Ar, and the mixture was heated to 150° C. for 90 min in a microwave reactor. The mixture was then filtered and the filtrate concentrated in vacuo. Purification by flash chromatography (SiO2, DCM/MeOH 99:1 to 90:10) gave the title compound (1.20 g) as a beige solid. UPLC-MS: MS 299.2 (M+H+); UPLC rt 0.85 min.

1. filtrationThe mixture was then filtered
2. concentrationthe filtrate concentrated in vacuo
3. customPurification by flash chromatography (SiO2, DCM/MeOH 99:1 to 90:10)