HRID2063730
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
Calcium trifluoromethanesulfonate (1.22 g, 3.60 mmol) was added to a solution of the product from stage 3 (2.51 g, 8.05 mmol) and 8-oxiranyl-1,4-dioxaspiro[4.5]decane (1.34 g, 7.30 mmol) in anhydrous tetrahydrofuran (50 ml) and the mixture was stirred at room temperature for 48 h. The tetrahydrofuran was removed i. vac. The residue was taken up in methylene chloride (40 ml) and the mixture was washed with 25% potassium carbonate solution (2×25 ml). The organic phase was dried with sodium sulfate and concentrated i. vac. The crude product (4.31 g) was purified by flash chromatography with cyclohexane/ethyl acetate (1:2).
WORKUP
后处理
- customThe tetrahydrofuran was removed i
- washthe mixture was washed with 25% potassium carbonate solution (2×25 ml)
- dry with materialThe organic phase was dried with sodium sulfate
- concentrationconcentrated i
- customThe crude product (4.31 g) was purified by flash chromatography with cyclohexane/ethyl acetate (1:2)