HRID928673

反应详情

EQUATION

反应方程式

HRID 928673 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

DMF (125 mL) was added to 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenol (8.46 g, 38 mmol), methyl 3-(bromomethyl)benzoate (8.8 g, 38 mmol), and potassium carbonate (10.6 g, 77 mmol), and stirred at room temperature overnight. The resultant was diluted with ethyl acetate, washed with water and saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure, and to the resulting residue, methanol (150 mL), water (30 mL), and lithium hydroxide (4.8 g, 114 mmol) were added, and stirred at room temperature overnight. After the solvent was distilled away under reduced pressure, the resultant was diluted with ethyl acetate, then washed with 1 N hydrochloric acid and saturated brine, and dried over anhydrous magnesium sulfate. After the solvent was distilled away under reduced pressure, the solid was collected by filtration.

WORKUP

后处理

  1. washwashed with water and saturated brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled away under reduced pressure
  4. stirringstirred at room temperature overnight
  5. distillationAfter the solvent was distilled away under reduced pressure
  6. additionthe resultant was diluted with ethyl acetate
  7. washwashed with 1 N hydrochloric acid and saturated brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationAfter the solvent was distilled away under reduced pressure
  10. filtrationthe solid was collected by filtration