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
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
Potassium carbonate (1.16 g, 8.39 mmol) was added to a solution of 5-fluoro-2-nitrotoluene (1.0 g, 6.45 mmol) and methyl salicylate (1.18 g, 7.74 mmol) in N,N-dimethylformamide (8 ml), and the resulting mixture was stirred at 140° C. for 1 hour. After the reaction, the reaction solution was cooled to 0° C. and a saturated aqueous sodium chloride solution was added thereto, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate. The organic layer dried was concentrated and then purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=10/1) to obtain methyl 2-(3-methyl-4-nitrophenoxy)benzoate (1.88 g, 85%).
WORKUP
后处理
- customAfter the reaction
- temperaturethe reaction solution was cooled to 0° C.
- extractionfollowed by extraction with ethyl acetate
- washThe organic layer was washed with water
- dry with materiala saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate
- customThe organic layer dried
- concentrationwas concentrated
- custompurified by a silica gel column chromatography (eluent: hexane/ethyl acetate=10/1)