反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 200 °C
PROCEDURE
实验过程
A suspension of 1-iodo-3-nitrobenzene (24.9 g, 0.1 mol), copper bronze (320 mg, 5 mmol) and potassium carbonate (15.2 g, 0.11 mol) in 2-pyrrolidinone was heated under a stream of nitrogen at 200° C. for 45 minutes. The reaction was cooled to ambient temperature, diluted with water (2000 ml) and extracted with diethyl ether (800 ml). The organic phase was then washed with water (2×800 ml), brine and dried over anhydrous sodium sulphate containing decolourising charcoal (2 g). Filtration and evaporation to dryness gave a yellow solid which was triturated with isohexane to give 1-(3nitrophenyl)pyrrolidin-2-one as a yellow powder (3.0 g, 15%). δH (360 MHz, CDCl3) 2.19-2.27 (2H, m), 2.67 (2H, t, J 8), 3.94 (2H, t, J 7), 7.54 (1H, t, J 8), 8.00 (1H, ddd, J 8, 2 and 1), 8.22 (1H, ddd, J 8, 2 and 1), 8.35 (1H, t, J 2).
WORKUP
后处理
- temperatureThe reaction was cooled to ambient temperature
- extractionextracted with diethyl ether (800 ml)
- washThe organic phase was then washed with water (2×800 ml), brine
- dry with materialdried over anhydrous sodium sulphate containing decolourising charcoal (2 g)
- filtrationFiltration and evaporation to dryness
- customgave a yellow solid which
- customwas triturated with isohexane