反应详情

温度

20 °C

To a solution of (E)-ethyl 3-((3aS,5aR,5bR,7aR,9S,11aR,11bR,13aS)-9-acetoxy-1-isopropyl-5a,5b,8,8,11a-pentamethyl-2-oxo-3,3a,4,5,5a,5b,6,7,7a,8,9,10,11,11a,11b,12,13,13a-octadecahydro-2H-cyclopenta[a]chrysen-3a-yl)-2-methylacrylate (2.0 g, 3.44 mmol) in THF (12 mL), MeOH (8 mL) and water (4 mL) was added sodium hydroxide (5.51 g, 138 mmol). The reaction mixture was stirred at 20° C. for 2 hrs. The reaction mixture was evaporated to dryness and the pH was adjusted to 5 with saturated NH4CI. The solid is solved into DCM (50 mL), washed with water, dried over Na2SO4 and concentrated to yield the (E)-3-((3aS,5aR,5bR,7aR,9S,11aR,11bR,13aS)-9-hydroxy-1-isopropyl-5a,5b,8,8,11a-pentamethyl-2-oxo-3,3a,4,5,5a,5b,6,7,7a,8,9,10,11,11a,11b,12,13,13a-octadecahydro-2H-cyclopenta[a]chrysen-3a-yl)-2-methylacrylic acid (1.3 g, 54.8%) as a yellow solid.

1. customThe reaction mixture was evaporated to dryness
2. washwashed with water
3. dry with materialdried over Na2SO4
4. concentrationconcentrated