HRID2167117
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
- 80 °C
PROCEDURE
实验过程
Potassium carbonate (1.12 g) was added to a solution of methyl 2,4-dihydroxybenzoate (454 mg) and 2-bromo-4,5-dimethoxybenzyl bromide (1.0 g) in dry acetone (80 ml). The reaction mixture was heated to reflux at 80° C. for 4 hours. The solvents were removed under vacuum and the residue was re-dissolved in DCM and washed with water (3×). The organic layer was passed through a hydrophobic frit and concentrated under vacuum. The crude residue was purified by chromatography on silica gel, eluting with petrol and increasing amounts of ethyl acetate.
WORKUP
后处理
- temperatureThe reaction mixture was heated
- customThe solvents were removed under vacuum
- dissolutionthe residue was re-dissolved in DCM
- washwashed with water (3×)
- concentrationconcentrated under vacuum
- customThe crude residue was purified by chromatography on silica gel
- washeluting with petrol
- temperatureincreasing amounts of ethyl acetate