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 (1500 mg, 2.76 mmol), 2-bromoethanol (1034 mg, 8.27 mmol), potassium phosphate (1756 mg, 8.27 mmol) and potassium iodide (916 mg, 5.52 mmol) in acetonitrile (10 mL) was heated to 120° C. for 15 h. The reaction mixture was poured into distilled water (40 mL). The white precipitate was filtered and washed with distilled water (100 mL). The white solid was dried under reduced pressure to provide the title compound (1.4 g, 86%), which was taken to the next step without further purification. LCMS: m/e 588.5 (M+H)+, 2.40 min (method 5).
WORKUP
后处理
- additionThe reaction mixture was poured
- distillationinto distilled water (40 mL)
- filtrationThe white precipitate was filtered
- washwashed with distilled water (100 mL)
- customThe white solid was dried under reduced pressure