反应详情

(3R)-(3,6-Dihydropyrazolo[4,3-d]pyrrolo[2,3-b]pyridin-1-yl)cyclopentanamine (0.12 g, 0.48 mmol, Preparation #29) and 2-cyanoacetic acid (0.042 g, 0.48 mmol), were combined in DMF (6.0 mL) with EDC (0.12 g, 0.65 mmol) and HOBt (0.076 g, 0.48 mmol). The mixture was stirred for about 3 h at room temperature. Perfluorophenyl 2-cyanoacetate (0.62 g, 2.5 mmol, Preparation #6) was added and the reaction mixture was stirred for about 48 h at room temperature. The solvent was removed under reduced pressure and the crude material was purified by RP-HPLC (Table 2, Method q) to give 2-cyano-N-((1R,3S)-3-(3,6-dihydropyrazolo[4,3-d]pyrrolo[2,3-b]pyridin-1-yl)cyclopentyl)acetamide (0.014 g, 9%): LC/MS (Table 2, Method a) Rt=1.52 min; m/z: 307 (M−H)−.

1. stirringthe reaction mixture was stirred for about 48 h at room temperature
2. customThe solvent was removed under reduced pressure
3. customthe crude material was purified by RP-HPLC (Table 2, Method q)