HRID1814122
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
- 22.5 °C
PROCEDURE
实验过程
To a solution of the compound obtained in Example 30 (3) (0.183 g) in a mixture of tetrahydrofuran (2 ml) and water (2 ml), OXONE (registered trademark) (0.4939 g) was added under ice-cooling and the mixture was stirred for 30 minutes and at 15 to 30° C. for 1.5 hours. A saturated aqueous sodium hydrogencarbonate solution was added thereto, and the mixture was extracted with ethyl acetate, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was separated using silica gel column chromatography (hexane:ethyl acetate=1:1) to obtain 0.1722 g of the desired product.
WORKUP
后处理
- additionwas added under ice-
- temperaturecooling
- extractionthe mixture was extracted with ethyl acetate
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe resulting residue was separated