反应详情

温度

100 °C

111-1. A mixture of 9-iodo-3,4,7,8-tetrahydro-[1,4]diazepino[7,1-a]isoquinoline-2,5-dione (440 mg, 1.24 mmol) in dry DCE (10 mL) was treated with POCl3 (0.23 mL, 2.49 mmol) and heated to 100° C. for 1 h. The mixture was allowed to cool to RT and then poured onto H2O and extracted with DCM. The combined org. layers were then dried over Na2SO4, filtered and concentrated in vacuo. The residue obtained was taken up in DCE (10 mL) and 4-ethyl-1H-imidazole (597 mg, 6.21 mmol) was added. The mixture was heated to 100° C. for 1 h. The mixture was then allowed to cool to RT, poured onto H2O, extracted with DCM and the combined org. layers were then dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by flash chromatography (SiO2, DCM to DCM/MeOH 9:1) to give the title compound (523 mg) as a brown oil. UPLC-MS: MS 433.1 (M+H+); UPLC rt 0.93 min.

1. temperatureto cool to RT
2. additionpoured onto H2O
3. extractionextracted with DCM
4. dry with materiallayers were then dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue obtained
8. temperatureThe mixture was heated to 100° C. for 1 h
9. temperatureto cool to RT
10. additionpoured onto H2O
11. extractionextracted with DCM
12. dry with materiallayers were then dried over Na2SO4
13. filtrationfiltered
14. concentrationconcentrated in vacuo
15. customThe crude product was purified by flash chromatography (SiO2, DCM to DCM/MeOH 9:1)