反应详情

温度

-50 °C

To a solution of 2,4-dichloro-phenol (15 g, 19.02 mmol) in toluene (200 ml) was added bromine (5.1 ml, 184.04 mmol) dropwise at −50° C. Then tert.-butylamine (19.4 ml, 99.02 mmol) was added dropwise and the reaction mixture was stirred at −50° C. for 30 minutes. The reaction was quenched by addition of 38% aqueous NaHSO3 solution, the organic layer was separated and the aqueous layer was extracted two times with EtOAc. The combined organic extracts were dried with Na2SO4, filtered and evaporated to obtain the title compound as white solid (21.5 g, 96%).

1. customThe reaction was quenched by addition of 38% aqueous NaHSO3 solution
2. customthe organic layer was separated
3. extractionthe aqueous layer was extracted two times with EtOAc
4. dry with materialThe combined organic extracts were dried with Na2SO4
5. filtrationfiltered
6. customevaporated