HRID1800605
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of tert-butyl(4-chloro-2-fluoro-5-hydroxyphenyl)carbamate (6.70 g, 25.6 mmol), 2-chloro-5-nitropyridine (4.06 g, 25.6 mmol), potassium carbonate (3.89 g, 28.1 mmol) and N,N-dimethylformamide (70 mL) was stirred at room temperature for 30 min. To the reaction mixture was added aqueous ammonium chloride solution (100 mL), and the mixture was extracted with ethyl acetate (150 mL×3). The organic layers were combined, and washed successively with water (100 mL) and saturated brine (50 mL), and dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give the title compound (4.52 g, 46%) as a white powder.
WORKUP
后处理
- extractionthe mixture was extracted with ethyl acetate (150 mL×3)
- washwashed successively with water (100 mL) and saturated brine (50 mL)
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure