反应详情

Into a 1 liter three-necked reaction vessel fitted with a cooling tube and a mechanical stirrer, 133 g (1.1 mols) of 2,4-dimethylphenylamine, 171 g (1.0 mol) of 1-bromo-4-methylbenzene, 11.2 g (0.05 mol) of palladium acetate, 32.4 g (0.2 mol) of 2-tert-butylphosphinoyl-2-methylpropane, 212 g (1.0 mol) of tripotassium phosphate and 500 mL of dimethylformamide were introduced to effect reflux for 12 hours in a nitrogen gas atmosphere and with heating in an oil bath. After the reaction was completed, the reaction mixture was left to cool to room temperature, followed by extraction with toluene/water, then washing with hydrochloric acid water, and thereafter distillation of the organic layer under reduced pressure to obtain the desired (2,4-dimethylphenyl)-p-tolylamine. The compound obtained was in a yield of 189.5 g corresponding to 84%. The compound obtained was measured with the same elementary analyzer as the above.

1. customInto a 1 liter three-necked reaction vessel fitted with a cooling tube and a mechanical stirrer
2. temperaturereflux for 12 hours in a nitrogen gas atmosphere
3. temperaturewith heating in an oil bath
4. waitthe reaction mixture was left
5. extractionfollowed by extraction with toluene/water
6. washwashing with hydrochloric acid water
7. distillationdistillation of the organic layer under reduced pressure