HRID887729
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
- 50 °C
PROCEDURE
实验过程
3-Amino-4-bromo-6-chloro-pyridine-2-carboxylic acid methyl ester (169 mg) was suspended in methanol (3 mL) and 2N sodium hydroxide solution (2 mL). The suspension was stirred at 50° C. for 3 hours. The precipitate was filtered off and washed carefully with diethyl ether. The precipitate was dissolved in a mixture of 2N hydrochloric acid and ethyl acetate and the layers were separated. The aqueous layer was 2× extracted with ethyl acetate, washed with brine, dried over MgSO4 and concentrated in vacuum to afford 138 mg of the title compound of the formula
WORKUP
后处理
- filtrationThe precipitate was filtered off
- washwashed carefully with diethyl ether
- dissolutionThe precipitate was dissolved in a mixture of 2N hydrochloric acid and ethyl acetate
- customthe layers were separated
- extractionextracted with ethyl acetate
- washwashed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuum