反应详情

To a 0° C. solution of 0.04 g (0.065 mmol) tert-butyl 2-[4-chloro-2-({[(5-chloro-2-{[2,2-difluoro-2-(2-pyridinyl)ethyl]amino}-3-fluoro-4-pyridinyl)acetyl]amino}methyl)phenyl]ethylcarbamate 1-10 in 2 mL EtOAc/1 mL MeOH was passed through a steady stream of HCl gas for 5 minutes, then the reaction mixture was concentrated to give N-[2-(2-aminoethyl)-5-chlorobenzyl]-2-(5-chloro-2-{[2,2-difluoro-2-(2-pyridinyl)ethyl]amino}-3-fluoro-4-pyridinyl)acetamide 1-11. 1H NMR (400 mHz, CD3OD) δ8.71 (d, 1H, J=4.58 Hz); 8.15 (apparent t, 1H, J=7.51 Hz); 7.89 (d, J=8.06 Hz); 7.70 (m, 2H); 7.29(d, 1H, J=1.84 Hz); 7.28 (dd, 1H, J=2.01 and 8.24 Hz); 7.23 (d, 1H, J=8,24 Hz); 4.42 (s, 2H); 4.36 (t, 2H, J=13.5 Hz); 3.80 (s, 2H); 3.41 (m, 2H); 3.02 (m, 2H). Mass Spectrum (electrospray) M+H=512.2

1. concentrationthe reaction mixture was concentrated