HRID1623700

反应详情

EQUATION

反应方程式

HRID 1623700 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureAfter the reaction mixture was cooled to room temperature
  2. customthe solvent was removed
  3. dissolutionthe residue was dissolved in water (100 ml)
  4. stirringstirred in an ice-water bath
  5. addition1N HCl (aq) was added
  6. filtrationThe solid was filtered
  7. dissolutiondissolved in ethyl acetate (80 ml)
  8. dry with materialThe solution was dried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure