反应详情

温度

0 °C

3-Amino-5-methoxy-pyridine (5.00 g, 40.3 mmol) was dissolved in THF (80 mL), cooled to 0° C., treated with pyridine (4.07 mL, 50.4 mmol) followed by phenylchloroformate (5.32 mL, 42.3 mmol). The reaction mixture was slowly warmed to RT over several hours and stirred an additional 12 h. The mixture was partitioned between water and EtOAc. The organic layer was separated and the aqueous layer was extracted again. The combined organic extracts were dried over sodium sulfate, filtered and concentrated to give the product as a reddish solid (9.45 g, 96%), which was used without purification.

1. temperatureThe reaction mixture was slowly warmed to RT over several hours
2. customThe mixture was partitioned between water and EtOAc
3. customThe organic layer was separated
4. extractionthe aqueous layer was extracted again
5. dry with materialThe combined organic extracts were dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated