反应详情

温度

95 °C

2,4-Difluoronitrobenzene (15.9 g; 0.10 mole), ethyl lactate (11.8 g; 0.10 mole), and anhydrous potassium carbonate (13.8 g, 0.10 mole) are combined in dioxane (200 ml) and the temperature is brought to 95° C. over a 1.5 hour period and maintained at 95° C. for 3 hours. The reaction mixture is cooled to room temperature, the inorganic solids removed by filtration and the solvent removed under vacuum to afford a dark colored oil, from which low boiling fractions are removed by distillation (bp., 79° C./0.5 mm). The pot residue is then cooled to afford 15.9 g of crude product, which is recrystallized from ligroin/acetone to afford ethyl 2-(5-fluoro-2-nitrophenoxy)propionate as yellow needles, m.p. 64°-65° C. Elemental anal. Calcd for C11H12FNO5 : C, 51.4; H, 4.70; F, 7.38; N, 5.45. Found: C, 51.35; H, 4.74; F, 7.60; N, 5.44.

1. temperatureThe reaction mixture is cooled to room temperature
2. customthe inorganic solids removed by filtration
3. customthe solvent removed under vacuum
4. customto afford a dark colored oil
5. customfrom which low boiling fractions are removed by distillation (bp., 79° C./0.5 mm)
6. temperatureThe pot residue is then cooled
7. customto afford 15.9 g of crude product, which
8. customis recrystallized from ligroin/acetone