HRID1881196
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
- -5 °C
PROCEDURE
实验过程
6-Hydroxy-5-methoxy-7-nitro-benzofuran-2-carboxylic acid ethyl ester (0.25 g) was dissolved to dichloromethane and cooled to −5° C. 1 M boron tribromide solution in dichloromethane (4.5 ml) was added and the mixture stirred at 0° C. for 24 hours. The mixture was poured in ice water and the dichloromethane layer separated. The water phase was extracted with ethyl acetate. The combined organic phases were dried with Na2SO4 and evaporated to dryness. The product was purified by reverse phase column chromatography using methanol (1%) in dichloromethane as an eluent.
WORKUP
后处理
- customthe dichloromethane layer separated
- extractionThe water phase was extracted with ethyl acetate
- dry with materialThe combined organic phases were dried with Na2SO4
- customevaporated to dryness
- customThe product was purified by reverse phase column chromatography