反应详情

温度

70 °C

To a solution of (9H-fluoren-9-yl)methyl 2-((3-(4-(2-hydroxypropan-2-yl)phenyl)-6-tosyl-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)methoxy)ethylcarbamate (0.030 g, 0.040 mmol, Preparation #AW.1) in 1,4-dioxane (1 mL) was added NaOH (5.0 N aqueous, 0.040 mL, 0.20 mmol). The mixture was heated at about 70° C. for about 4 h. The mixture was then concentrated under reduced pressure, dissolved in MeOH/DMSO (1:1) (2 mL) and purified via reverse phase preparatory HPLC (Table 2, Method n). The desired fractions were collected and concentrated under reduced pressure. The residue was dissolved in water (4 mL) and lyophilized for 16 h to give 2-(4-(1-((2-aminoethoxy)methyl)-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-3-yl)phenyl)propan-2-ol (6.5 mg, 44%): LC/MS (Table 2, Method a) Rt=1.30 min.; MS m/z: 364 (M−H)−.

1. concentrationThe mixture was then concentrated under reduced pressure
2. dissolutiondissolved in MeOH/DMSO (1:1) (2 mL)
3. custompurified via reverse phase preparatory HPLC (Table 2, Method n)
4. customThe desired fractions were collected
5. concentrationconcentrated under reduced pressure
6. dissolutionThe residue was dissolved in water (4 mL)