反应详情

温度

0 °C

N-(tert-butoxycarbonyl)-3-cyclopropyl-D-alanyl-N-[5-chloro-2-(1H-1,2,4-triazol-1-yl)benzyl]-L-prolinamide from the previous step (0.058 g, 0.112 mmol) was dissolved in EtOAc (2 mL) and cooled with stirring to 0° C. HCl/EtOAc (3.55M, 1.5 mL) was added. The bath was removed and the mixture stirred for 2 hours. HPLC analysis indicated completion and the solvent was removed under reduced pressure. The residue was triturated with EtOAc and filtered to give the hydrochloride salt of 3-cyclopropyl-D-alanyl-N-[5-chloro-2-(1H-1,2,4-triazol-1-yl)benzyl]-L-prolinamide as a solid. (0.045 g). HPLC RT=1.04 min, Method B; LCMS (M+H): 417, 419; 1H NMR (400 MHz, DMSO-d6): δ 8.96, (s, 1H), 8.67 (t, J=6 Hz, 1H), 8.27–8.33 (m, 3H), 7.50–7.56 (m, 3H), 4.32 (dd, J=2, 9 Hz, 1H), 4.10–4.25 (m, 2H), 3.78–3.86 (m, 1H), 3.54–3.60 (m, 1H), 2.06–2.11 (m, 1H), 1.81–1.93 (m, 3H), 1.68–1.75 (m, 1H, 154–1.60 (m, 1H), 0.77–0.85 (m, 1H), 0.44–0.48 (m, 2H), 0.07–0.16 (m, 2H).

1. temperaturecooled
2. customThe bath was removed
3. stirringthe mixture stirred for 2 hours
4. customthe solvent was removed under reduced pressure
5. customThe residue was triturated with EtOAc
6. filtrationfiltered