HRID494529
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
A solution of Example 33B (0.052 g, 0.112 mmol), mesyl chloride (0.035 mL, 0.447 mmol), and pyridine (0.073 mL, 0.893 mmol) in acetone (1.5 mL) was stirred at 25° C. for 18 hours. The solution was partitioned between ethyl acetate and dilute citric acid and the layers were separated. The ethyl acetate layer was dried with sodium sulfate, filtered, and concentrated in vacuo. The residue was chromatographed on silica gel eluting with methylene chloride and 2.5% methanol in methylene chloride to give the desired product (0.054 g, 96%).
WORKUP
后处理
- customThe solution was partitioned between ethyl acetate and dilute citric acid
- customthe layers were separated
- dry with materialThe ethyl acetate layer was dried with sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was chromatographed on silica gel eluting with methylene chloride and 2.5% methanol in methylene chloride