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
4-Methoxy-N-[4-(2-pyrrolidin-1-yl-ethoxy)-phenyl]-N-[4-(tetrahydro-pyran-2-yloxy)-benzyl]-benzenesulfonamide (1.58 g, 2.79 mmol) was suspended in 3:1 ethanol:1N HCl (30 mL) and the solution was stirred at room temperature for 24 hr. The reaction mixture was quenched with sodium bicarbonate solution and the aqueous solution was washed with methylene chloride. The organic layer was dried (sodium sulfate), filtered, and concentrated to a white solid. The crude material was purified via Biotage® (A Dynax Corp., Charlottesville, Va.) chromatography using 10% methanol/methylene chloride as the eluant. The purified material was suspended in methanol (15 mL) and 4.0M HCl in dioxane (1.5 equiv.) was added. The mixture was stirred at room temperature and was concentrated to dryness to yield the title compound as the HCl salt. MS 483.1 (M+1)+
WORKUP
后处理
- customThe reaction mixture was quenched with sodium bicarbonate solution
- washthe aqueous solution was washed with methylene chloride
- dry with materialThe organic layer was dried (sodium sulfate)
- filtrationfiltered
- concentrationconcentrated to a white solid
- customThe crude material was purified via Biotage® (A Dynax Corp
- concentrationwas concentrated to dryness