HRID1492629
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 solution of 2.34 g (7.45 mmol) of the product of Step J in DMF (30 mL) were added imidazole (609 mg, 8.94 mmol) and tertbutyldimethyl-chlorosilane (1.35 g, 8.94 mmol) at 0° C. The solution was stirred at room temperature for 18 hours, and was then poured into 100 mL of ethyl acetate and washed with H2O (2×). The water layer was extracted with ethyl acetate (2×). The combined organic layer was washed with H2O (3×) and brine, and was dried over anhydrous MgSO4. After concentration the mixture was purified by flash chromatography (hexane: EtOAc=10:1) to give 1.96 g of the title compound as a clear oil.
WORKUP
后处理
- washwashed with H2O (2×)
- extractionThe water layer was extracted with ethyl acetate (2×)
- washThe combined organic layer was washed with H2O (3×) and brine
- dry with materialwas dried over anhydrous MgSO4
- concentrationAfter concentration the mixture
- customwas purified by flash chromatography (hexane: EtOAc=10:1)