反应详情

温度

60 °C

To a solution of 2,4,6-trimethylbenzyl chloride (5 g, 29.7 mmol) in DMSO (20 mL) was added sodium azide (2.9 g, 44.6 mmol). The mixture was heated at 60° C. for 3 h before it was allowed to cool to rt and poured to water (200 mL). The resulted precipitate was filtered dissolved in wet THF (50 mL) followed by the addition of triphenylphosphine (15.6, 59.4 mmol). The mixture was heated under reflux for 3 h and the volatiles were evaporated. The residue was added to 1 N HCl (200 mL) and the solids were filtered off. The filtrate was basified and the resulted precipitate was filtered, dried under vacuum to give 2,4,6-trimethylbenzylamine (2.7 g, 61% yleld).

1. temperatureto cool to rt
2. filtrationThe resulted precipitate was filtered
3. dissolutiondissolved in wet THF (50 mL)
4. temperatureThe mixture was heated
5. temperatureunder reflux for 3 h
6. customthe volatiles were evaporated
7. additionThe residue was added to 1 N HCl (200 mL)
8. filtrationthe solids were filtered off
9. filtrationthe resulted precipitate was filtered
10. customdried under vacuum