反应详情

温度

50 °C

A mixture of (R)-3-[{N-(2-(tert-butoxycarbonylamino)-5-trifluoromethylbenzoyl}glycyl)amino]-1-(4-chlorobenzyl)pyrrolidine (6.3 g, 11.4 mmol), Pd(OH)2 (1.68 g), HCO2H (3.7 mL), and methanol (80 mL) was stirred at 50° C. overnight. After the mixture was cooled to room temperature, the Pd catalyst was filtered off through Celite and the filtrate was concentrated. Column chromatography (SiO2, AcOEt, AcOEt/MeOH=5/1-4/1) gave (R)-3-[{N-2-(tert-butoxycarbonylamino)-5-trifluoromethylbenzoyl}glycyl]aminolpyrrolidine (4.42 g, 90%) as a white solid: 1H NMR (CDCl3, 400 MHz) δ1.48 (s, 9 H), 2.0-2.4 (m, 2 H), 3.42-3.71 (m, 5 H), 4.00-4.22 (m, 2 H), 4.56 (br, 1 H), 7.48 (d, J=9.0 Hz, 1 H), 7.93 (s, 1 H), 8.17 (br, 1 H), 8.33 (d, J=9.0 Hz, 1 H), 8.45 (br, 1 H).

1. temperatureAfter the mixture was cooled to room temperature
2. filtrationthe Pd catalyst was filtered off through Celite
3. concentrationthe filtrate was concentrated
4. customColumn chromatography (SiO2, AcOEt, AcOEt/MeOH=5/1-4/1) gave (R)-3-[{N-2-(tert-butoxycarbonylamino)-5-trifluoromethylbenzoyl}glycyl]aminolpyrrolidine (4.42 g, 90%) as a white solid