HRID533661
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
- 105 °C
PROCEDURE
实验过程
To a mixture of 3-nitro-5-trifluoromethylpyridin-2-ol (3.2 g) and DMF (1 drop), phosphorous oxychloride (8.2 ml) was added at room temperature. The mixture was heated to 105° C., and stirred with heating for 2 days. The reaction mixture was cooled to room temperature, and then the reaction mixture was poured into ice, and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure to give 2.5 g of 2-chloro-3-nitro-5-trifluoromethylpyridine.
WORKUP
后处理
- additionwas added at room temperature
- temperaturewith heating for 2 days
- temperatureThe reaction mixture was cooled to room temperature
- additionthe reaction mixture was poured into ice
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated under reduced pressure