反应详情

温度

80 °C

A mixture of methyl 4-((1R,3aS,5aR,5bR,7aR,11aS,11bR,13aR,13bR)-3a-((2-(4-(cyclopropylsulfonyl)piperazin-1-yl)ethyl)amino)-5a,5b,8,8,11a-pentamethyl-1-(prop-1-en-2-yl)-2,3,3a,4,5,5a,5b,6,7,7a,8,11,11a,11b,12,13,13a,13b-octadecahydro-1H-cyclopenta[a]chrysen-9-yl)benzoate (30 mg, 0.039 mmol) and sodium hydroxide (0.395 mL, 0.395 mmol) in dioxane (0.5 mL) was heated up at 80° C. for 3 hours. The reaction mixture was filtered and the clear solution was purified by HPLC to provide the title compound as a white solid (13 mg, 42%). LCMS: m/e 746.58 (M+H)+, 2.27 min (method 11). 1H NMR (400 MHz, Acetic) δ 7.99 (d, J=8.3 Hz, 2H), 7.26 (d, J=8.3 Hz, 2H), 5.34 (d, J=4.8 Hz, 1H), 4.81 (s, 1H), 4.70 (s, 1H), 3.63-3.44 (m, 5H), 3.43-3.26 (m, 2H), 3.24-3.13 (m, 1H), 3.05 (d, J=4.3 Hz, 4H), 2.86 (br. s., 1H), 2.58-2.40 (m, 1H), 2.27-1.02 (m, 22H), 1.73 (s, 3H) 1.24 (s, 3H), 1.13 (d, J=4.5 Hz, 2H), 1.10 (s, 3H), 1.06 (s, 3H), 1.02 (d, J=4.5 Hz, 2H), 0.97 (s, 3H), 0.96 (s, 3H).

1. filtrationThe reaction mixture was filtered
2. customthe clear solution was purified by HPLC