HRID747868
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 a solution of 7-methoxy-3-(6-methoxy-pyridin-3-yl)-4-methyl-chromen-2-one in CH2Cl2 (5 mL) at room temperature was added BBr3 (1.0 N, 24.2 mmoL, 24 mL) dropwise. After addition, the reaction was slightly heated to reflux 4 hours. The reaction was quenched with ice sat. NaHCO3, extracted with 3×CH2Cl2, washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to give the crude material. The crude material was re-crystallized in 2:1 hexanes:ethyl acetate to afford the title product as a pale reddish solid.
WORKUP
后处理
- additionAfter addition
- temperaturethe reaction was slightly heated
- temperatureto reflux 4 hours
- customThe reaction was quenched with ice sat. NaHCO3
- extractionextracted with 3×CH2Cl2
- washwashed with brine
- dry with materialdried over anhydrous Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customto give the crude material
- customThe crude material was re-crystallized in 2:1 hexanes