反应详情

N,N-Dimethyl-5-ethyl-2-(2′-bromo-4′-chloro-6′-fluoroanilino)phenylacetamide (2.5 g, 6.0 mmol) is combined with DMF (10 ml), triethylamine (10 ml), tri-o-tolylphosphine (0.5 g, 1.6 mmol), tetramethyltin (4 ml, 5.16g, 28.9 mmol) and palladium acetate (0.25 g, 1.1 mmol), and the mixture heated in a sealed tube for 3 days at 95°. The tube is allowed to cool and carefully opened. Water and ethyl acetate are added to the reaction and the mixture separated. The organic fraction is washed with a dilute NaCl solution (2×50 ml). The combined aqueous fractions are then washed with ethyl acetate and the combined organic fractions are then dried (magnesium sulfate). The material is absorbed onto a small amount of silica gel and purified by flash chromatography (on silica, ethyl acetate:hexanes, 1:4 to 1:1) to give N,N-dimethyl-5-ethyl-2-(4′-chloro-2′-fluoro-6′-methylanilino)phenylacetamide.

1. temperaturethe mixture heated in a sealed tube for 3 days at 95°
2. temperatureto cool
3. customthe mixture separated
4. washThe organic fraction is washed with a dilute NaCl solution (2×50 ml)
5. washThe combined aqueous fractions are then washed with ethyl acetate
6. dry with materialthe combined organic fractions are then dried (magnesium sulfate)
7. customThe material is absorbed onto a small amount of silica gel
8. custompurified by flash chromatography (on silica, ethyl acetate:hexanes, 1:4 to 1:1)