反応 #52600
ord-a060504d193f467db215cf91a13afa3f
反応条件
温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度The mixture was cooled to room temperature
- 2温度The mixture was heated at 100° C. for 2 hours
- 3温度cooled
- 4その他quenched with 300 mL of saturated ammonium chloride solution
- 5抽出The mixture was extracted three times with ethyl acetate
- 6洗浄the combined organic layers washed with water and brine
- 7その他evaporated
実験手順
Dimethyl malonate (10 mL) in 25 mL of dimethylsulfoxide was added dropwise to 3.5 g sodium hydride suspended in 25 mL dimethylsulfoxide and the mixture heated at 100° C. for 10 minutes. The mixture was cooled to room temperature and 4.7 g of 4-fluoro-3-nitrobiphenyl in 25 mL dimethylsulfoxide was added. The mixture was heated at 100° C. for 2 hours, cooled and quenched with 300 mL of saturated ammonium chloride solution. The mixture was extracted three times with ethyl acetate and the combined organic layers washed with water and brine and evaporated to give, as a yellow oil, crude dimethyl-3-nitrobiphenyl-4-malonate.