反应详情

温度

20 °C

A mixture of (3R,4R)-4-[(R)-7-(2-fluoro-phenyl)-4-methyl-3-oxo-2,3,4,10-tetrahydro-9-oxa-1,2,4a-triaza-phenanthren-6-yl]-3-methyl-piperidine-1-carboxylic acid tert-butyl ester (0.076 g, 0.149 mmol) in HCl (4M in EtOAc, 15 mL) was stirred at 20° C. for 1 h. The reaction mixture was concentrated in vacuo to give (R)-7-(2-fluoro-phenyl)-4-methyl-6-((3R,4R)-3-methyl-piperidin-4-yl)-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one hydrochloride acid (0.065 g, 98%). 1H NMR (MeOD, 400 MHz) δ 7.50-7.41 (m, 1H), 7.32-7.19 (m, 3H), 6.91 (brs, 1H), 6.86 (s, 1H), 4.80 (m, 1H), 4.70-4.59 (m, 2H), 3.48 (m, 1H), 3.15-2.98 (m, 2H), 2.82 (m, 1H), 2.43 (m, 1H), 1.88 (m, 2H), 1.50 (d, J=6.4 Hz, 3H), 0.91 (brs, 3H). LC/MS (Table 1, Method 4) Rt=1.534 min.; MS m/z: 409 [M+H]+. SFC (Table 1, Method 43), Rt=1.341 min.

1. concentrationThe reaction mixture was concentrated in vacuo