HRID2086068

反应详情

EQUATION

反应方程式

HRID 2086068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureThe reaction was cooled to ambient temperature
  2. extractionextracted with diethyl ether (800 ml)
  3. washThe organic phase was then washed with water (2×800 ml), brine
  4. dry with materialdried over anhydrous sodium sulphate containing decolourising charcoal (2 g)
  5. filtrationFiltration and evaporation to dryness
  6. customgave a yellow solid which
  7. customwas triturated with isohexane