反应详情

A mixture of 4-(2-methyl-2-nitropropyl)phenol (3.0 g, 15.4 mmol), ethylbromoacetate (2.04 mL, 17.0 mmol) and potassium carbonate (6.4 g, 46.2 mmol) was stirred at room temperature for 18 h. The reaction was concentrated in vacuo and the resulting residue partitioned between EtOAc and water. The layers were separated and the aqueous layer extracted with EtOAc (3×). The combined organic layers were washed with water (3×), brine, dried (Na2SO4), and concentrated in vacuo to a brown oil. The material was purified by flash chromatography over silica gel eluting with 5% MeOH/CHCl3 to provide 4.22 g (97%) of a clear oil. NMR

1. concentrationThe reaction was concentrated in vacuo
2. customthe resulting residue partitioned between EtOAc and water
3. customThe layers were separated
4. extractionthe aqueous layer extracted with EtOAc (3×)
5. washThe combined organic layers were washed with water (3×), brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo to a brown oil
8. customThe material was purified by flash chromatography over silica gel eluting with 5% MeOH/CHCl3