反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
A mixture of methyl 4-((1R,3aS,5aR,5bR,7aR,11aS,11bR,13aR,13bR)-5a,5b,8,8,11a-pentamethyl-3a-((2-(piperazin-1-yl)ethyl)amino)-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 (50 mg, 0.076 mmol), 2-(1H-benzo[d][1,2,3]triazol-1-yl)-1,1,3,3-tetramethylisouronium tetrafluoroborate (29.4 mg, 0.091 mmol), N-ethyl-N-isopropylpropan-2-amine (11.82 mg, 0.091 mmol) and 2-(dimethylamino)-2-oxoacetic acid (26.8 mg, 0.229 mmol) in dichloromethane (2 mL) was stirred at 20° C. for 2 hours. The reaction mixture was diluted with distilled water (5 mL), extracted with ethyl acetate (3×4 mL), the extracts were combined, dried over sodium sulfate, filtered and concentrated under reduced pressure to provide the desired product as a yellow oil (40 mg, 70%). LCMS: m/e 755.68 (M+H)+, 2.42 min (method 11).
WORKUP
后处理
- extractionextracted with ethyl acetate (3×4 mL)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure