HRID714045
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
The crude sodium 4-bromo-6-(methoxycarbonyl)-5H-cyclopenta[c]pyridin-7-olate (20.0 mmol) was dissolved in aq. 6 M HCl, (54 mL) and heated at reflux for 1.5 h. The acidic solution was cooled in ice, poured into Et2O, basified with aq. 6 M KOH (to give a pH of −9) and extracted with Et2O (2×). The Et2O phases were collected, dried over Na2SO4, concentrated and purified by flash chromatography (20 g SiO2, i-PrOH (1%)/CH2Cl2) to afford after trituration with a small amount of Et2O the title compound (0.69 g, 16% over 2 steps) as pink solid. MS: 212.0 (M+H−, 1 Br).
WORKUP
后处理
- temperatureheated
- temperatureat reflux for 1.5 h
- temperatureThe acidic solution was cooled in ice
- customto give a pH of −9) and
- extractionextracted with Et2O (2×)
- customThe Et2O phases were collected
- dry with materialdried over Na2SO4
- concentrationconcentrated
- custompurified by flash chromatography (20 g SiO2, i-PrOH (1%)/CH2Cl2)