反应详情

温度

75 °C

To a solution of tert-butyl 4-((1R,3aS,5aR,5bR,7aR,11aS,11bR,13aR,13bR)-3a-((N-(2-(dimethylamino)ethyl)-4-methoxy-4-oxobutanamido)methyl)-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 (53 mg, 0.068 mmol) in 1,4-dioxane (1 ml) was added NaOH (0.338 ml, 0.338 mmol). The mixture was heated to 75° C. for 3 h. The mixture was cooled to rt and was quenched with 1N HCl (3 ml) and extracted with dichloromethane (3×7 ml). The combined organic layers were dried with Na2SO4, were filtered, and concentrated under reduced pressure. The crude product was used in the next step with no additional purification. LCMS: m/e 771.6 (M+H)+, 2.70 min (method 6).

1. temperatureThe mixture was cooled to rt
2. customwas quenched with 1N HCl (3 ml)
3. extractionextracted with dichloromethane (3×7 ml)
4. dry with materialThe combined organic layers were dried with Na2SO4
5. filtrationwere filtered
6. concentrationconcentrated under reduced pressure
7. customThe crude product was used in the next step with no additional purification
8. customm/e 771.6 (M+H)+, 2.70 min (method 6)