HRID1358115

反应详情

EQUATION

反应方程式

HRID 1358115 的结构方程式

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

  1. temperaturecooled to −78°
  2. extractionThe mixture was extracted with ether, which
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. custompurified on silica gel eluting with 8% ethyl acetate in CH2Cl2