反应详情

温度

82 °C

A mixture of methyl 4-((1R,3aS,5aR,5bR,7aR,11aS,11bR,13aR,13bR)-3a-((2-(4-(2-(dimethylamino)-2-oxoacetyl)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 (40 mg, 0.053 mmol) and sodium hydroxide (0.530 mL, 0.530 mmol) in dioxane (1 mL) was heated up at 82° C. for 3 hours. The reaction mixture was cooled to room temperature, filtered and the clear solution was purified by HPLC to provide the title compound as a white solid (17 mg, 41%). LCMS: m/e 741.65 (M+H)+, 2.29 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), 5.33 (d, J=4.5 Hz, 1H), 4.82 (s, 1H), 4.71 (s, 1H), 4.14-3.78 (m, 2H), 3.75-3.36 (m, 6H), 3.22 (br. s., 4H), 3.03 (s, 3H), 3.00 (s, 3H), 2.92-2.75 (m, 1H), 2.29-1.05 (m, 22H), 1.73 (s, 3H), 1.20 (s, 3H), 1.10 (s, 3H), 1.05 (s, 3H), 0.98 (s, 3H), 0.96 (s, 3H).

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered
3. customthe clear solution was purified by HPLC