反应详情

A mixture of 2-(3-bromo-4-fluorobenzoyl)-3-methoxymethoxypyridine (5.68 g), 3.6N-sulfuric acid (6.0 mL) and acetone (30 mL) was refluxed for 3 hours. The reaction mixture was then poured into water, neutralized with a saturated aqueous solution of sodium hydroxide, and extracted 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 purified by means of a silica gel column (ethyl acetate--hexane) to afford 2-(3-bromo-4-fluorobenzoyl)-3-hydroxypyridine (4.51 g) (compound C-5). Physical properties and spectrum date of the product are shown in Table 5 and Table 6.

1. temperaturewas refluxed for 3 hours
2. extractionextracted 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 purified by means of a silica gel column (ethyl acetate--hexane)