反应详情

To a solution of 3-methylpyrrolidine-1,3-dicarboxylic acid 1-tert-butyl ester (348 mg, 1.52 mmol) in DMF (10 mL) were added DIPEA (0.53 mL, 3.04 mmol), pyrrolidine (0.25 mL, 3.04 mmol) and HATU (693 mg, 1.82 mmol). The reaction mixture was stirred at room temperature for 18 hours and then partitioned between water and EtOAc. The organic layer was separated and washed with a 0.1N aqueous HCl solution and brine, dried over Na2SO4, filtered and concentrated to give the desired product as a white solid (334 mg, 78%). 1H NMR (400 MHz, CHCl3-d): δ 3.61-3.38 (m, 8H); 2.00-1.79 (m, 6H); 1.47-1.44 (m, 9H); 1.33 (s, 3H).

1. custompartitioned between water and EtOAc
2. customThe organic layer was separated
3. washwashed with a 0.1N aqueous HCl solution and brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated