反应详情

A mixture of 7.8 g (0.032 mole) of 2-chloro-4-fluoro-5-diacetylaminotoluene, 6.2 g (0.035 mole) of N-bromosuccinimide, 0.5 g of benzoyl peroxide, and 200 ml of carbon tetrachloride was heated at reflux for two days. This mixture was filtered, and the filtrate was washed with water. The filtrate was dried, and the solvent was evaporated under reduced pressure. The residue was passed through a column of silica gel, eluting with ethyl acetate/heptane (1/4). Appropriate fractions were combined, and the solvent was evaporated under reduced pressure, yielding 0.82 g of 2-chloro-4-fluoro-5-diacetylaminobenzyl bromide. The nmr was consistent with the proposed structure.

1. temperaturewas heated
2. temperatureat reflux for two days
3. filtrationThis mixture was filtered
4. washthe filtrate was washed with water
5. customThe filtrate was dried
6. customthe solvent was evaporated under reduced pressure
7. washeluting with ethyl acetate/heptane (1/4)
8. customthe solvent was evaporated under reduced pressure