反应详情

A mixture of 2-(3-bromo-4-fluorobenzoyl)-3-hydroxypyridine (1.26 g), O-t-butylhydroxylamine hydrochloride (1.08 g) and ethanol (10 mL) was refluxed for 2 hours. The reaction mixture was poured into water, and subjected to extraction with ethyl acetate. The extract was washed with water and a saturated aqueous saline solution, successively, and dried (sodium sulfate), followed by evaporating the solvent under reduced pressure. The residue was subjected to purification by means of a silica gel column (ethyl acetate--hexane) to afford (E)-2-(3-bromo-α-t-butoxyimino-4-fluorobenzyl)-3-hydroxypyridine (0.89 g) and (Z)-2-(3-bromo-α-t-butoxyimino-4-fluorobenzyl)-3-hydroxypyridine (0.51 g) (compounds 17 and 16).

1. temperaturewas refluxed for 2 hours
2. extractionsubjected to extraction with ethyl acetate
3. washThe extract was washed with water
4. dry with materiala saturated aqueous saline solution, successively, and dried (sodium sulfate)
5. customby evaporating the solvent under reduced pressure
6. customThe residue was subjected to purification by means of a silica gel column (ethyl acetate--hexane)