反应详情

温度

90 °C

4-(6-Bromo-2-(4-methoxybenzylamino)quinolin-3-yl)tetrahydro-2H-pyran-4-ol (0.250 g, 0.564 mmol) in a mixture of dioxane (4 mL), 5N HCl (4.00 mL, 20.00 mmol) and concentrated HCl (1.00 mL, 32.9 mmol) was heated at 90° C. for 5 h. The reaction was transferred to a microwave reaction vessel and heated in a microwave reactor at 130° C. for 40 min and was concentrated. The crude solid was partitioned between EtOAc and 10% sodium carbonate. The combined organic extracts were washed with water, saturated sodium chloride, and dried over sodium sulfate. The solution was filtered and concentrated in vacuo to give the crude material. The crude material was purified by silica gel chromatography by eluting with 1:30 2M NH3 in MeOH/DCM to provide 6-bromo-3-(3,6-dihydro-2H-pyran-4-yl)quinolin-2-amine as white solid.

1. customThe reaction was transferred to a microwave reaction vessel
2. temperatureheated in a microwave reactor at 130° C. for 40 min
3. concentrationwas concentrated
4. customThe crude solid was partitioned between EtOAc and 10% sodium carbonate
5. washThe combined organic extracts were washed with water, saturated sodium chloride
6. dry with materialdried over sodium sulfate
7. filtrationThe solution was filtered
8. concentrationconcentrated in vacuo
9. customto give the crude material
10. customThe crude material was purified by silica gel chromatography
11. washby eluting with 1:30 2M NH3 in MeOH/DCM