反应详情

温度

0 °C

To a stirred solution of 5-bromo-3-pyridinamine (0.8 g, 4.62 mmol), triethylamine (2.6 mL, 18.48 mmol) in dichloromethane (20 mL) at 0° C. under inert atmosphere. The reaction mixture was stirred for 15 min and then ethyl sulfonyl chloride (0.88 mL, 9.24 mmol) was added slowly. The reaction mixture was stirred for 2 h at room temperature. Diluted with dichloromethane and then washed with saturated aqueous sodium chloride solution, separated the organic layer, dried over sodium sulphate, concentrated under high vacuum, light yellow solid obtained. The solid was dissolved in methanol (10 mL), cooled to 0° C., added 10N aqueous sodium hydroxide (10 mL) solution. The reaction mixture was stirred for 1 h and then methanol was evaporated completely and extracted with ethyl acetate. The combined organic layer was washed with saturated aqueous sodium chloride solution, dried over sodium sulphate and concentrated under vacuum to obtain the title compound. MS (M+1): 266.9.

1. customat 0° C.
2. stirringThe reaction mixture was stirred for 2 h at room temperature
3. washwashed with saturated aqueous sodium chloride solution
4. customseparated the organic layer
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated under high vacuum, light yellow solid
7. customobtained
8. stirringThe reaction mixture was stirred for 1 h
9. custommethanol was evaporated completely
10. extractionextracted with ethyl acetate
11. washThe combined organic layer was washed with saturated aqueous sodium chloride solution
12. dry with materialdried over sodium sulphate
13. concentrationconcentrated under vacuum