反应详情

温度

20 °C

To a stirring solution of (R)-1-cyclopropyl-3-(3-fluoro-4-(4-(3-methylmorpholino)-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-2-yl)phenyl)urea hydrochloride (intermediate 33) (112 mg, 0.25 mmol) in DMF (2 ml), was added Et3N (70 μL, 0.5 mmol). Reaction mixture was stirred at room temperature (20° C.) for 2 minutes followed by the addition of cyclopropanecarbonyl chloride (23 μL, 0.25 mmol) followed by stirring at room temperature for two hours. The reaction mixture was concentrated in vacuo before partitioning between water (10 ml) and DCM (10 ml). The organic layer was recovered, passed through a hydrophobic frit and the solvent removed in vacuo. Residue was then purified by prep. HPLC at high pH to afford the title compound as an off white solid (25 mg, 0.052 mmol, 21%).

1. customReaction mixture
2. stirringby stirring at room temperature for two hours
3. concentrationThe reaction mixture was concentrated in vacuo
4. custombefore partitioning between water (10 ml) and DCM (10 ml)
5. customThe organic layer was recovered
6. customthe solvent removed in vacuo
7. customResidue was then purified by prep