反应详情

温度

140 °C

100-1. A mixture of 9-iodo-3,4,7,8-tetrahydro-[1,4]diazepino[7,1-a]isoquinoline-2,5-dione (150 mg, 0.42 mmol), tributyl(1-ethoxyvinyl)stannane (153 mg, 0.42 mmol) and Pd(PPh3)4 (49 mg, 0.04 mmol) in dioxane (3 mL) was heated to 140° C. for 2 h in a microwave reactor. The mixture was then concentrated in vacuo and the residue obtained was purified by flash chromatography (SiO2, heptane to AcOEt to AcOEt/MeOH 85:15) afforded the compound obtained was taken up in THF (20 mL) and treated with a 2M aqueous solution of HCl (0.68 mL, 1.36 mmol). The solution was stirred at RT for 1 h and then concentrated in vacuo. The residue obtained was taken up in a saturated aq. solution of NaHCO3 and extracted with DCM. The combined org. layers were then dried over Na2SO4, filtered and concentrated in vacuo to give the title compound (79 mg). UPLC-MS: MS 271.2 (M+H+); UPLC rt 0.59 min.

1. concentrationThe mixture was then concentrated in vacuo
2. customthe residue obtained
3. customwas purified by flash chromatography (SiO2, heptane to AcOEt to AcOEt/MeOH 85:15)
4. customafforded the compound
5. customobtained
6. concentrationconcentrated in vacuo
7. customThe residue obtained
8. extractionextracted with DCM
9. dry with materiallayers were then dried over Na2SO4
10. filtrationfiltered
11. concentrationconcentrated in vacuo