HRID1171200
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 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
- extractionfollowed by extraction with ethyl acetate
- washThe organic layer was washed with water and sat. NaCl
- dry with materialby drying over anhydrous magnesium sulfate
- filtrationfiltering
- concentrationThe filtrate was concentrated under a reduced pressure
- customthe residue was purified by silica gel column chromatography (heptane:ethyl acetate=4:1)