反应详情

温度

105 °C

5-Methyl-2-pyridinecarboxylic acid 1-oxide (0.9 g, 5.88 mmol) was added to phosphoryl trichloride (30 mL). The mixture was stirred at 105° C. for 3 h. After that the mixture was cooled to room temperature, added to ice water slowly and extracted with methylene chloride (4×30 mL). The organic layer was washed with brine (50 mL), dried over anhydrous sodium sulfate, and concentrated to give the crude product (0.85 g, 84.3%); MS (EI): m/e=172.0 [M+H]+.

1. temperatureAfter that the mixture was cooled to room temperature
2. extractionextracted with methylene chloride (4×30 mL)
3. washThe organic layer was washed with brine (50 mL)
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated