反应详情

4.0 g (17 mmol) of 3-fluoro-2-methyl-4-(methylsulfonyl)benzoic acid were dissolved in 12.9 ml (172 mmol) of allylamine. The mixture was heated at reflux for 5 days and allowed to stand for 2 days. 10 ml (134 mmol) of allylamine and 15 ml of water were added, and the mixture was heated at reflux for 14 days, cooled to RT, added to ice, acidified with 10% strength sulfuric acid and extracted twice with ethyl acetate. The combined organic phases were dried over MgSO4, and the solvent was removed under reduced pressure. The residue was crystallized from diethyl ether. This gave 4.2 g of a yellow solid of a purity of 88%.

1. temperatureThe mixture was heated
2. temperatureat reflux for 5 days
3. temperaturethe mixture was heated
4. temperatureat reflux for 14 days
5. additionadded to ice
6. extractionextracted twice with ethyl acetate
7. dry with materialThe combined organic phases were dried over MgSO4
8. customthe solvent was removed under reduced pressure
9. customThe residue was crystallized from diethyl ether