反应详情

温度

180 °C

6-chloro-5-methyl-pyridine-2-carboxylic acid (0.85 g, 4.97 mmol) and sodium sulfite (CAN 7757-83-7, 1.5 g, 11.9 mmol) were added to water (3 mL) and ethanol (3 mL). The mixture was heated to 180° C. for 4 h in a sealed tube. After that the mixture was cooled to room temperature and a solid precipitated that was removed by filtration. The filtrate was concentrated and added to water (20 mL). The aqueous phase was washed with ethyl acetate (2×20 mL). Subsequently the aqueous phase was adjusted to pH=2 with 2 N hydrochloric acid. Water was removed in vacuo to give the product as solid (1.2 g); MS (EI): m/e=218.0 [M+H]+.

1. temperatureAfter that the mixture was cooled to room temperature
2. customa solid precipitated that
3. customwas removed by filtration
4. concentrationThe filtrate was concentrated
5. additionadded to water (20 mL)
6. washThe aqueous phase was washed with ethyl acetate (2×20 mL)
7. customWater was removed in vacuo