反应详情

温度

0 °C

25 g (134 mmol) of 2-bromo-4-aminotoluene are placed in 400 ml of 1M sulfuric acid in a round-bottomed flask, and the mixture is then cooled to 0° C. 13 g (190 mmol) of sodium nitrite dissolved in 30 ml of water are added, followed by addition of 21 ml of concentrated sulfuric acid. The mixture is refluxed for 4 hours. It is then extracted with ethyl ether. The organic phase is dried over magnesium sulfate, filtered and then evaporated. The residue obtained is purified by chromatography on a column of silica eluted with a mixture of heptane and ethyl acetate (90/10) to give 12.1 g (48%) of the expected product in the form of a brown oil.

1. additionare added
2. temperatureThe mixture is refluxed for 4 hours
3. extractionIt is then extracted with ethyl ether
4. dry with materialThe organic phase is dried over magnesium sulfate
5. filtrationfiltered
6. customevaporated
7. customThe residue obtained
8. customis purified by chromatography on a column of silica
9. washeluted with a mixture of heptane and ethyl acetate (90/10)