반응 #1904043

반응 방정식

4,4′-diiodobiphenyl

potassium carbonate

N-phenyl-2-naphthylamine

DMF

→

beta-NPD

수율 72.4%

용매

water

반응 조건

후처리

1. 1
   온도It was heated at 200 degrees Centigrade
2. 2
   온도refluxed for 12 hours until no peaks of starting materials and intermediates
3. 3
   workup.ADDITIONto disperse
4. 4
   여과It was filtrated
5. 5
   세척washed with water
6. 6
   기타Precipitated crystals
7. 7
   기타were purified by silica gel column chromatography

실험 절차

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.

출처