反应详情

温度

60 °C

To a solution of 4-bromo-2-nitro-phenol (3.28 g, 15.0 mmol, 1 equiv) in dimethylformamide (40 mL) at 23° C. was added potassium carbonate (4.14 g, 30 mmol, 2 equiv) followed by ethyl bromoacetate (1.84 mL, 16.6 mmol, 1.1 equiv). The resulting mixture was warmed to 60° C. (oil bath) for 90 min then cooled to 23° C. The reaction mixture was partitioned between ethyl acetate:heptane (1:1) and water (100 mL each). The organic layer was separated and washed successively with water, saturated brine solution (100 ml, each) then dried (MgSO4), filtered and concentrated to give 4.50 g (11.5 mmol, 77%) of the product as a yellow oil.

1. temperaturethen cooled to 23° C
2. customThe reaction mixture was partitioned between ethyl acetate:heptane (1:1) and water (100 mL each)
3. customThe organic layer was separated
4. washwashed successively with water, saturated brine solution (100 ml
5. dry with materialeach) then dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated