HRID1171200

反应详情

EQUATION

反应方程式

HRID 1171200 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an N,N-dimethylformamide (100 mL) solution of 2,5-dihydroxybenzaldehyde (10.0 g, 72.4 mmol) were added sodium hydride (5.79 g, 145 mmol) and benzyl bromide (18.9 mL, 159 mmol) at 0° C., which was stirred at room temperature for 24 hours. Water was added to the reaction solution at 0° C. followed by extraction with ethyl acetate. The organic layer was washed with water and sat. NaCl, followed by drying over anhydrous magnesium sulfate and filtering. The filtrate was concentrated under a reduced pressure and the residue was purified by silica gel column chromatography (heptane:ethyl acetate=4:1) to obtain the title compound (17.6 g, 76%) as a white solid.

WORKUP

后处理

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with water and sat. NaCl
  3. dry with materialby drying over anhydrous magnesium sulfate
  4. filtrationfiltering
  5. concentrationThe filtrate was concentrated under a reduced pressure
  6. customthe residue was purified by silica gel column chromatography (heptane:ethyl acetate=4:1)