反应详情

温度

105 °C

A mixture of 12.0 g (51.7 mmol) 6-chloro-2-ethylsulfanyl-4-methyl-pyridine-3-carboxylic acid and 33.7 g (387 mmol) morpholine was heated to 105° C. for 5 d. After cooling to RT a 2M aq. NaOH sol. (200 ml) was added, followed by washing with ether (3×200 ml). The aqueous layer was then acidified with a 2M aq. HCl to pH 5 and extracted with EtOAc. In the same manner pH 4 was adjusted followed by extraction with EtOAc. The combined EtOAc extracts were dried over MgSO4 and concentrated in vacuo. Crystallisation (DCM/hexane) of the residue yielded 7.2 g (25.3 mmol, 49%) 2-ethylsulfanyl-4-methyl-6-morpholin-4-yl-pyridine-3-carboxylic acid.

1. additionwas added
2. washby washing with ether (3×200 ml)
3. extractionextracted with EtOAc
4. extractionIn the same manner pH 4 was adjusted followed by extraction with EtOAc
5. dry with materialThe combined EtOAc extracts were dried over MgSO4
6. concentrationconcentrated in vacuo
7. customCrystallisation (DCM/hexane) of the residue