反应详情

温度

50 °C

A mixture of 2-chloro-4-fluoro-5-nitrophenol (100 g), anhydrous potassium carbonate (86.6 g) and dimethylformamide (500 g) was heated at 50° C., and amyl 2-chloroacetate (90.2 g) was dropwise added thereto in 30 minutes, followed by allowing to stand at 60° C. for 4 hours. The reaction mixture was cooled to room temperature, and water (1500 g) was added thereto, followed by extraction with ethyl acetate (1500 g). The organic layer was separated, washed with water and concentrated under reduced pressure. The residue was distilled under reduced pressure to give 4-chloro-2-fluoro-5-(pentyloxycarbonylmethyloxy)nitrobenzene (Compound (III)) (129 g) as a pale yellow oil. Yield, 77%. b.p., 160 °-165° C./0.7 mmHg.

1. waitto stand at 60° C. for 4 hours
2. temperatureThe reaction mixture was cooled to room temperature
3. extractionfollowed by extraction with ethyl acetate (1500 g)
4. customThe organic layer was separated
5. washwashed with water
6. concentrationconcentrated under reduced pressure
7. distillationThe residue was distilled under reduced pressure