反应详情

温度

20 °C

To a solution of methyl 4-((1R,3aS,5aR,5bR,7aR,11aS,11bR,13aR,13bR)-3a-((2-aminoethyl)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 (15 mg, 0.026 mmol) and Hunig's Base (0.013 mL, 0.077 mmol) in dichloromethane (1 mL) was added methanesulfonyl chloride (3.81 mg, 0.033 mmol) in dichloromethane (1 mL). The reaction mixture was stirred at 20° C. for 2 hours. The reaction mixture was diluted with distilled water (3 mL), extracted with dichloromethane (3×3 mL), the extracts were combined, dried over sodium sulfate, filtered and concentrated under reduced pressure to provide the desired product as a yellow solid (15 mg, 88%). LCMS: m/e 665.55 (M+H)+, 2.44 min (method 11).

1. extractionextracted with dichloromethane (3×3 mL)
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure