反应详情

温度

60 °C

3-(Benzyloxy)-6-(4,5-dihydro-1H-imidazol-2-yl)-2-methoxyaniline (Step 7, 30 g, 93 mmol) was added portionwise over 1 h to a round bottom flask containing TFA (400 mL) precooled with an ice bath. The reaction mixture was heated to 60° C. and allowed to stir at this temperature for 17 h at which time it was cooled to rt and the reaction mixture concentrated under reduced pressure. The resulting residue was taken up in DCM and hexanes and concentrated under reduced pressure. The material thus obtained was dissolved in MeOH and DCM (250 mL, 1:1) and concentrated under reduced pressure. The resulting solid was dried overnight under vacuum with low heat to give the title compound (100%): 1H NMR (DMSO-d6) δ: 7.61 (1H, m), 6.87 (1H, m), 4.15 (2H, br t), 4.00 (2H, m), 3.64 (3H, s).

1. customprecooled with an ice bath
2. temperaturewas cooled to rt
3. concentrationthe reaction mixture concentrated under reduced pressure
4. concentrationhexanes and concentrated under reduced pressure
5. customThe material thus obtained
6. concentrationDCM (250 mL, 1:1) and concentrated under reduced pressure
7. customThe resulting solid was dried overnight under vacuum
8. temperaturewith low heat