反应详情

温度

80 °C

To a mixture of 1.25 mL (10.5 mmol) tert-butyl nitrite and 1.42 g (10.5 mmol) copper(II)chloride in 40 mL acetonitrile was added a solution of 1.20 g (6.59 mmol) 4-amino-6-methoxy-pyridine-2-carboxylic acid methyl ester in 10 mL acetonitrile dropwise at 40° C. This mixture was stirred at 80° C. for 1 h, then poured into ice water, acidified with 4 M aqueous HCl and extracted with EtOAc. The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo. The crude material was purified by flash chromatography (PE/EtOAc=3/1→2/1).

1. extractionextracted with EtOAc
2. dry with materialThe combined organic phases were dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude material was purified by flash chromatography (PE/EtOAc=3/1→2/1)