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
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
Solid LiOH (0.79 g, 18.77 mmol) was added to a stirred solution of phenylmethyl 2-[(phenylmethyl)oxy]-5-(4-pyridinyl)benzoate (may be prepared as described in Description 78; 0.81 g, 1.88 mmol) in tetrahydrofuran (50 ml) and water (10 ml) in air at room temperature. The reaction mixture was stirred at 70° C. overnight. After the reaction mixture was cooled to room temperature, the solvent was removed and the residue was dissolved in water (100 ml) and stirred in an ice-water bath. 1N HCl (aq) was added to adjust the pH to 4. The solid was filtered, and dissolved in ethyl acetate (80 ml). The solution was dried over Na2SO4, filtered, and concentrated under reduced pressure to yield the title compound as a white solid, 486 mg.
WORKUP
后处理
- temperatureAfter the reaction mixture was cooled to room temperature
- customthe solvent was removed
- dissolutionthe residue was dissolved in water (100 ml)
- stirringstirred in an ice-water bath
- addition1N HCl (aq) was added
- filtrationThe solid was filtered
- dissolutiondissolved in ethyl acetate (80 ml)
- dry with materialThe solution was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure