反应 #1904043

反应方程式

4,4′-diiodobiphenyl

potassium carbonate

N-phenyl-2-naphthylamine

DMF

→

beta-NPD

收率 72.4%

溶剂

water

反应条件

后处理

1. 1
   温度It was heated at 200 degrees Centigrade
2. 2
   温度refluxed for 12 hours until no peaks of starting materials and intermediates
3. 3
   workup.ADDITIONto disperse
4. 4
   过滤It was filtrated
5. 5
   洗涤washed with water
6. 6
   其他Precipitated crystals
7. 7
   其他were purified by silica gel column chromatography

实验过程

25.1 g (61.5 mmol) of 4,4′-diiodobiphenyl, 2.14 g of poly(ethylene glycol) PEG-6000 that was available from Wako Pure Chemical Industries, Ltd., 17.1 g (0.124 mol) of potassium carbonate and 15.7 g (247 mmol) of powdered copper were added to 32.4 g (148 mmol) of N-phenyl-2-naphthylamine. It was heated at 200 degrees Centigrade. It was determined for tracing by the high-speed liquid chromatography. And it was stirred and refluxed for 12 hours until no peaks of starting materials and intermediates were determined. DMF and water were added thereto to disperse. It was filtrated and washed with water. Precipitated crystals were purified by silica gel column chromatography to obtain 26.2 g of beta-NPD that is represented by Compound Example 5 at 72.4% yield.

来源