HRID1751527
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
- 110 °C
PROCEDURE
实验过程
A mixture of 1-(5-bromo-2-iodobenzyloxy)-6-methoxynaphthalene (5.0 g, 10.7 mmol) and sodium acetate (2.64 g, 32.1 mmol) in dimethylformamide (100 mL) was degassed with a stream of argon for 15 minutes. PdCl2(PPh3)2 was added and the reaction was heated to 110° C. After 16 hours the reaction was diluted with ethyl acetate, washed with water and brine, dried (Na2SO4) and concentrated. The resulting residue was purified by flash column chromatography to yield 8-bromo-2-methoxy-6H-dibenzo[c,h]chromene (1.29 g, 35%).
WORKUP
后处理
- customwas degassed with a stream of argon for 15 minutes
- additionPdCl2(PPh3)2 was added
- additionAfter 16 hours the reaction was diluted with ethyl acetate
- washwashed with water and brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customThe resulting residue was purified by flash column chromatography