反応 #1904043

反応方程式

4,4′-diiodobiphenyl

potassium carbonate

N-phenyl-2-naphthylamine

DMF

→

beta-NPD

収率 72.4%

溶媒

water

反応条件

後処理

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
   ろ過It was filtrated
5. 5
   洗浄washed with water
6. 6
   その他Precipitated crystals
7. 7
   その他were purified by silica gel column chromatography

実験手順

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.

出典