反応 #2384561
ord-2d69693921f947ef9869edd189980690
反応方程式
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度was refluxed for 15 hours
- 2温度The reaction mixture was cooled
- 3抽出extracted with ethyl acetate
- 4濃縮The extract was concentrated
- 5抽出The product was extracted with ethyl acetate
- 6その他purified by silica gel chromatography
実験手順
A solution comprised of sodium iodide (7.9 g, 52.7 mmol) and 2-chloroethyl phenyl sulfide (4.7 g, 27.2 mmol) in acetone (40 mL) was refluxed for 15 hours. The reaction mixture was cooled, diluted with ice water and extracted with ethyl acetate. The extract was concentrated and the residue was combined with N-methylpyrrolidone (20 mL), lithium hydroxide (1.6 g, 67 mmol) and diethyl 2-benzoylaminomalonate (5 g, 18 mmol). The mixture was stirred at ambient temperature of 15 hours and then poured into cold water. The product was extracted with ethyl acetate and purified by silica gel chromatography to provide diethyl 2-benzoylamino-2-(2-phenylsulfanylethyl)malonate (1.316 g, 3.2 mmol).