反应详情

A mixture of (Z)-2-(3-bromo-α-t-butoxyimino-4-fluorobenzyl)-3-hydroxypyridine (0.55 g), 70% m-chloro perbenzoic acid (0.74 g) and tetrahydrofuran (10 mL) was stirred overnight at room temperature. To the reaction mixture was added an aqueous solution of sodium sulfite. The reaction mixture was stirred for 30 minutes, and subjecting to extraction with ethyl acetate. The extract was washed with water and a saturated aqueous saline solution, successively, and dried (sodium sulfate) and then concentrated. The concentrate was crystallized from isopropyl ether, and recrystallized from ethanol-water to afford (Z)-2-(3-bromo-α-t-butoxyimino-4-fluorobenzyl)-3-hydroxypyridine 1-oxide (0.46 g) (compound 25).

1. stirringThe reaction mixture was stirred for 30 minutes
2. extractionsubjecting 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. concentrationconcentrated
6. customThe concentrate was crystallized from isopropyl ether
7. customrecrystallized from ethanol-water