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
- 0 °C
PROCEDURE
实验过程
Sodium bis(2-methoxyethoxy)aluminum hydride (65 wt % solution in toluene, 1.2 mL, 4 mmol) was added to a solution of 4-{4-[1-ethyl-1-(4-hydroxy-3-methyl-phenyl)-propyl]-2-methyl-phenylethynyl}-tetrahydro-thiopyran-4-ol (Example 136-(1); 0.54 g, 1.3 mmol) in tetrahydrofuran (6 mL) in a nitrogen atmosphere at 0° C., and the mixture was stirred at 0° C. for five hours. Then, ethyl acetate and brine were added to the reaction mixture, which was further diluted with ethyl acetate. Thereafter, celite was added and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (hexane:ethyl acetate=100:0 to 25:75) to give the target compound as a colorless oil (0.5 g, 92%).
WORKUP
后处理
- additionThereafter, celite was added
- stirringthe mixture was stirred at room temperature for 30 minutes
- filtrationThe reaction mixture was filtered through celite
- concentrationthe filtrate was concentrated under reduced pressure
- customThe resulting residue was purified by silica gel chromatography (hexane:ethyl acetate=100:0 to 25:75)