反应详情

1-(2-Aminomethyl-4-chloro-phenyl)-pyrrolidin-2-one: To 5-chloro-2-fluorobenzonitrile (0.3 g, 1.929 mmol) and pyrrolidin-2-one (0.246 g, 2.89 mmol) in DMF (5 mL) was added NaH (0.116 g, 2.89 mmol) and the reaction was stirred overnight. The reaction mixture was partitioned with EtOAc/water/brine and extracted with EtOAc. The combined organic layers were washed with water and brine, dried (MgSO4), and evaporated to give 5-Chloro-2-(2-oxo-pyrrolidin-1-yl)-benzonitrile (0.42 g). LCMS m/z 221.2 (M+H)+. This intermediate was converted to 125A following the procedure described for 102B. LCMS m/z 207.2 (M+H—NH3)+. 1HNMR (400 MHz, CHLOROFORM-D) δ: 2.08-2.20 (m, 2 H) 2.57 (t, J=7.71 Hz, 2 H) 3.56 (t, J=6.69 Hz, 2 H) 4.61 (s, 2 H) 6.50 (d, J=8.34 Hz, 1 H) 6.97 (d, J=2.27 Hz, 1 H) 7.11 (dd, J=8.34, 2.27 Hz, 1 H).

1. customThe reaction mixture was partitioned with EtOAc/water/brine
2. extractionextracted with EtOAc
3. washThe combined organic layers were washed with water and brine
4. dry with materialdried (MgSO4)
5. customevaporated