反应详情

Ethyl 4-fluoro-2-hydroxybenzoate (10.2 g, 55 mmol)) was dissolved in n-heptane. Iodo monochloride (12 g, 74 mmol) was added dropwise at ambient temperature with stirring. After 1 h, water was added and then solid sodium sulfite in small portions until the suspension was decolourized. More n-heptane was added to clear solution and the phases separated. The organic phase was dried and concentrated. The product crystallized on cooling. It was collected by filtration and washed with cold n-heptane. The crude yield was 10 g. The product was a mixture of ethyl 4-fluoro-2-hydroxy-5-iodobenzoate (about 80%) and the 5 chloro analogue (about 20%).

1. customthe phases separated
2. customThe organic phase was dried
3. concentrationconcentrated
4. customThe product crystallized
5. temperatureon cooling
6. filtrationIt was collected by filtration
7. washwashed with cold n-heptane
8. additiona mixture of ethyl 4-fluoro-2-hydroxy-5-iodobenzoate (about 80%)