反应详情

A solution of 5-(cyclopropylamino)-6-(cyclopropylmethoxy)-pyridine-2-carboxylic acid methyl ester (400 mg, 1.53 mmol), sodium hydroxide (244 mg, 6.1 mmol) in THF/H2O 1/1 (10 mL) was stirred for 1 h at room temperature. The reaction mixture was concentrated under reduced pressure. Water was added and the pH was adjusted to 2 by addition of 1 N HCl. Extraction with ethyl acetate (30 mL) was followed by washing with brine (6×30 mL). The organic layer was dried over sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography (silica gel, 50 g, 50% ethyl acetate in petroleum ether) to yield the title compound (350 mg, 92%) as yellow solid; MS (EI): m/e=249.3 [M+H]+.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionWater was added
3. additionthe pH was adjusted to 2 by addition of 1 N HCl
4. extractionExtraction with ethyl acetate (30 mL)
5. washby washing with brine (6×30 mL)
6. dry with materialThe organic layer was dried over sodium sulfate
7. concentrationconcentrated in vacuo
8. customThe residue was purified by column chromatography (silica gel, 50 g, 50% ethyl acetate in petroleum ether)