反应详情

温度

20 °C

A mixture of 3-methyl-3-((R)-1-methyl-2-oxo-8-vinyl-1,2,3,5-tetrahydro-6-oxa-3,4,10,11 b-tetraaza-cyclopenta[b]phenanthren-10-yl)-azetidine-1-carboxylic acid tert-butyl ester (0.08 g, 0.177 mmol) and 10% Pd/C (0.002 g, 0.018 mmol) in methanol (2 mL) was stirred under an atmosphere of H2 at 20° C. for 2.5 h. The mixture was filtered and the filtrate was evaporated in vacuo. The residue was purified by prep-HPLC (Table 3, Method 32) to give 3-((R)-8-ethyl-1-methyl-2-oxo-1,2,3,5-tetrahydro-6-oxa-3,4,10,11b-tetraaza-cyclopenta[b]phenanthren-10-yl)-3-methyl-azetidine-1-carboxylic acid tert-butyl ester (0.04 g, 49%) as a gum. 1H NMR (400 MHz, methanol-d4): δ 7.18 (s, 1H), 7.00 (s, 1H), 6.81 (s, 1H), 4.98 (m, 1H), 4.61-4.47 (m, 4H), 4.27 (m, 2H), 2.70 (q, J=7.6 Hz, 2H), 1.77 (s, 3H), 1.50-1.47 (m, 12H), 1.32 (m, J=7.6 Hz, 3H). LC/MS (Table 1, Method 25) Rt=0.896 min.; MS m/z: 454 [M+H]+.

1. filtrationThe mixture was filtered
2. customthe filtrate was evaporated in vacuo
3. customThe residue was purified by prep-HPLC (Table 3, Method 32)