HRID1971759
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
PROCEDURE
实验过程
To a cooled (−60° C.) solution of 800 mg 19d in 10 mL THF was added 2.04 mmol n-butyllithium. After stirring at −60° C. for 30 min 877 mg N-fluorobenzenesulfonimide was added. The mixture was allowed to reach room temperature and was stirred for another 2 h. Water was added and the mixture was extracted with 2×ethyl acetate. The combined organic phases were dried and concentrated. The crude product by column chromatography over silica to afford an oil, which was crystallized from heptane/diisopropyl ethyl ether to give compound 340 mg of 27a as a pale yellow solid.
WORKUP
后处理
- additionwas added
- customto reach room temperature
- extractionthe mixture was extracted with 2×ethyl acetate
- customThe combined organic phases were dried
- concentrationconcentrated
- customThe crude product by column chromatography over silica to afford an oil, which
- customwas crystallized from heptane/diisopropyl ethyl ether