HRID1948

反应详情

EQUATION

反应方程式

HRID 1948 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

33.85 g (0.2 mol) of 5-aminoacenaphtthene was mixed with 102.1 g (0.5 mol) of iodo benzene, 1.3 g (0.02 mol) of copper powder, 34.5 g (0.25 mol) of anhydrous potassium carbonate and 100 ml of nitrobenzene, and the mixture was stirred at 200° C. for 26 hours. The reaction was determined to be finished when disappearance of 5-aminoacenaphthene and 5-(N-phenylamino)acenaphthene as an intermediate was identified. 300 ml of toluene was added thereto to dissolve a product, and the resultant mixture was filtrated and concentrated. The concentrated product was purified by column chromatography (carrier: silica gel, eluent: toluene/hexane=1/4) to obtain 48.7 g (yield: 75.7%, melting point: 168.5°-170.5° C.) of 5-(N,N-diphenylamino)acenaphthene.

WORKUP

后处理

  1. dissolutionto dissolve a product
  2. filtrationthe resultant mixture was filtrated
  3. concentrationconcentrated
  4. customThe concentrated product was purified by column chromatography (carrier: silica gel, eluent: toluene/hexane=1/4)