反应详情

To a solution of 3,5-dibromo-4-methylaniline (4.17 g, 15.74 mmol) in CH2I2 (10 mL) was added tert-butylnitrite (3.0 mL, 23.61 mmol) slowly at 0° C. while stirring vigorously. The ice bath was removed and the reaction mixture was stirred at rt while the reaction was very exothermic, then placed in 80° C. oil bath and heated for 20 min. CH2I2 was distilled off under high vacuum, and the remaining residue was purified by flash chromatography eluting with 100% hexane to give the title compound.

1. customThe ice bath was removed
2. stirringthe reaction mixture was stirred at rt while the reaction
3. customplaced in 80° C.
4. temperatureheated for 20 min
5. distillationCH2I2 was distilled off under high vacuum
6. customthe remaining residue was purified by flash chromatography
7. washeluting with 100% hexane