反应详情

To a solution of 1-(4-(5-isopropyl-1H-pyrazol-3-ylamino)-6,7-dihydro-5H-cyclopenta[d]pyrimidin-2-yl)pyrrolidine-2-carboxylic acid (5 g, 14 mmol) in MeOH (120 mL) was added HOBt.H2O (143 mg, 0.94 mmol), N-methylmorpholine (1.42 g, 14 mmol) and EDC.HCl (3.64 g, 19 mmol). The reaction mixture was stirred at RT overnight. The MeOH was removed under reduced pressure and the residue was dissolved in EtOAc (100 mL). The solution was washed with water (2×40 mL) followed by brine (40 mL) and dried over anhydrous sodium sulfate. Removal of EtOAc under reduced pressure afforded methyl 1-(4-(5-isopropyl-1H-pyrazol-3-ylamino)-6,7-dihydro-5H-cyclopenta[d]pyrimidin-2-yl)pyrrolidine-2-carboxylate, Compound (iv) (5 g, 96% yield). 1H NMR (400 MHz, CDCl3) δ (ppm): 1.30 (d, 6H), 1.98-2.20 (m, 4H), 2.06-2.37 (m, 1H), 2.60-2.66 (m, 2H), 2.67-2.2.88 (m, 2H), 2.90-3.07 (m, 1H), 3.65-3.79 (m, 1H), 3.70 (s, 3H), 3.80-3.91 (m, 2H), 4.61-4.70 (m, 1H), 6.18 (s, 1H), 6.59 (s, 1H).

1. customThe MeOH was removed under reduced pressure
2. dissolutionthe residue was dissolved in EtOAc (100 mL)
3. washThe solution was washed with water (2×40 mL)
4. dry with materialdried over anhydrous sodium sulfate
5. customRemoval of EtOAc under reduced pressure