反应详情

A solution of 2-(5-bromo-2-hydroxybenzoyl)-3-(1,3-dioxolan-2-yl)pyridine (2.92 g), O-t-butyl-hydroxylamine hydrochloride (2.09 g) and pyrrolidine (1.78 g) in n-propanol (40 ml) was heated for 2 hours under reflux. The reaction mixture was concentrated, to which was added water, followed by subjecting the mixture to extraction with ethyl acetate. The extract solution was washed with a saturated aqueous saline solution, dried (anhydrous sodium sulfate), and concentrated. The concentrate was purified by means of a silica gel column chromatography (eluent: ethyl acetate/hexane) to give (Z)-2-(5-bromo-2-hydroxybenzoyl)-3-(1,3-dioxolan-2-yl)pyridine O-t-butyloxime (2.81 g) (Compound 134).

1. temperatureunder reflux
2. concentrationThe reaction mixture was concentrated, to which
3. additionwas added water
4. extractionto extraction with ethyl acetate
5. washThe extract solution was washed with a saturated aqueous saline solution
6. dry with materialdried (anhydrous sodium sulfate)
7. concentrationconcentrated
8. customThe concentrate was purified by means of a silica gel column chromatography (eluent: ethyl acetate/hexane)