HRID494597
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 the product of Example 49-5 (185.0 g, 0.334 mol) in dichloromethane (220 mL) was added 4 M HCl in dioxane (430 mL, 1.72 mol) and the solution was mixed at room temperature for 3.5 h. The reaction was quenched by addition of ethyl acetate (1 L) and pH 7 phosphate buffer (1.5 L) and the layers were separated. The organic layer was concentrated and chased with ethanol to a final volume of approximately 1100 mL. The product precipitated and was isolated by filtration and dried to give the title compound (105.79 g, 70%).
WORKUP
后处理
- additionthe solution was mixed at room temperature for 3.5 h
- customThe reaction was quenched by addition of ethyl acetate (1 L) and pH 7 phosphate buffer (1.5 L)
- customthe layers were separated
- concentrationThe organic layer was concentrated and chased with ethanol to a final volume of approximately 1100 mL
- customThe product precipitated
- customwas isolated by filtration
- customdried