反应详情

5-Aminopyridine-2-carboxylic acid (1.60 g, 11.6 mmol) was dissolved in MeOH (100 mL) and concentrated sulfuric acid (1.7 mL, 12.8 mmol) was added and the mixture was heated to 80 C for 5 hours. The reaction mixture was concentrated under vacuum, neutralised by adding 1M aq. sodium bicarbonate and extracted with EtOAc. The organic layer was dried over sodium sulfate and concentrated under vacuum to afford the title compound as a pale yellow solid (1.813 g, quant.). Method B HPLC-MS: MH+ requires m/z=153 Found: m/z=153, Rt=0.35 min (by MS).

1. temperaturethe mixture was heated to 80 C for 5 hours
2. concentrationThe reaction mixture was concentrated under vacuum
3. additionby adding 1M aq. sodium bicarbonate
4. extractionextracted with EtOAc
5. dry with materialThe organic layer was dried over sodium sulfate
6. concentrationconcentrated under vacuum