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
- 120 °C
PROCEDURE
实验过程
A mixture of 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 (50 mg, 0.092 mmol), 3-((2-chloroethyl)amino)tetrahydrothiophene 1,1-dioxide (45.4 mg, 0.230 mmol), potassium phosphate (58.5 mg, 0.276 mmol) and potassium iodide (30.5 mg, 0.184 mmol) in acetonitrile (1 mL) was heated up at 120° C. for 18 hours. The reaction mixture was quenched with distilled water (3 mL), extracted with dichloromethane (3×3 mL), the organic phases were combined, dried over sodium sulfate, filtered and concentrated under reduced pressure to provide the crude product as a white solid (40 mg, 62%). LCMS: m/e 705.48 (M+H)+, 2.44 min (method 11).
WORKUP
后处理
- customThe reaction mixture was quenched with distilled water (3 mL)
- extractionextracted with dichloromethane (3×3 mL)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure