반응 단계
The title compound was prepared in 26% yield from methyl 4-((1R,3aS,5aR,5bR,7aR,11aS,11bR,13aR,13bR)-3a-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 following the same procedure as described for the preparation of 4-((1R,3aS,5aR,5bR,7aR,11aS,11bR,13aR,13bR)-3a-(3-(dimethylamino)propanamido)-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)benzoic acid, except 4-(dimethylamino)butyric acid hydrochloride was used instead of 3-(dimethylamino)propionic acid hydrochloride in Step 1. LCMS: m/e 643.4 (M+H)+, 4.19 min (method 8). 1H NMR (500 MHz, METHANOL-d4) δ=7.95 (d, J=8.2 Hz, 2H), 7.24 (d, J=8.5 Hz, 2H), 5.33 (dd, J=1.7, 6.3 Hz, 1H), 4.80 (d, J=1.5 Hz, 1H), 4.67 (s, 1H), 3.21-3.14 (m, 2H), 2.93 (s, 6H), 2.82-2.67 (m, 2H), 2.49 (t, J=6.9 Hz, 2H), 2.41 (dd, J=8.2, 12.2 Hz, 1H), 2.18 (dd, J=6.4, 17.1 Hz, 1H), 2.06-1.96 (m, 3H), 1.96-1.86 (m, 1H), 1.85-1.79 (m, 1H), 1.77 (br. s., 1H), 1.75 (s, 3H), 1.73-1.69 (m, 1H), 1.64-1.56 (m, 3H), 1.55-1.48 (m, 4H), 1.47-1.38 (m, 3H), 1.35 (d, J=12.2 Hz, 1H), 1.33-1.27 (m, 1H), 1.21-1.17 (m, 1H), 1.15 (s, 3H), 1.12 (d, J=3.4 Hz, 1H), 1.07 (s, 6H), 0.99 (s, 3H), 0.97 (s, 3H).
