HRID1358115
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
CONDITIONS
反应条件
- 温度
- -5 °C
PROCEDURE
实验过程
A solution of Example 5C (5.44 g., 15.72 mmole) in THF (70 mL) and cooled to −5° C. was treated with of 1.8M phenyllithium in ether-cyclohexane (52.4 mL, 94.33 mmol). The mixture was stirred at −5° C. for 1 hour, cooled to −78° and a solution of aqueous KHCO3 was added rapidly. The mixture was extracted with ether, which was combined, dried (Na2SO4), filtered, concentrated under reduced pressure and purified on silica gel eluting with 8% ethyl acetate in CH2Cl2 to provide the titled compound (4.84 g, 85% yield).
WORKUP
后处理
- temperaturecooled to −78°
- extractionThe mixture was extracted with ether, which
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- custompurified on silica gel eluting with 8% ethyl acetate in CH2Cl2