实在是做不出来了,求同行指导？ tetrahedron volume 54, issue 16, 16 april 1998, pages 4107-4124 biphenyl 2,2',6,6'-tetracarboxylicacid (5). to pyrene (6.00 g, 29.7 mmol) in ch2ci 2 (120 ml) was added mecn (120 ml) and water (180 ml). to the resulting biphasic solution was added naio 4 (60 g, 280 mmol) followed by ru(iii)cl 3 (240 mg, 1.16 mmol). the solution warmed somewhat as the reaction began but was not vigorous. the reaction was run overnight (~ 16 h) with stirring and was filtered to give a yellow solid. the mixed solid (tetraacid/nalo4) was extracted with acetone (750 ml) and the acetone was refiitered to yield a yellow solution. upon evaporation the product was identified as a mixture of the desired tetraacid and the corresponding dianhydride. the crude product was ground to a fine powder and was refluxed for 1 h in ch2ci 2 before being filtered hot. the tetraacid was collected as a white powder (7.4 g, 75% yield), m. p. 300 ° c. ~h nmr (dmso-d 6, 300 mhz) 5 12.4 (br s, 4 h), 7.96 (d, j= 7.6 hz, 4 h), 7.45 (t, j-- 7.8 hz, 2 h). 四酸與產物應該都會一起出來 , 可以利用溶解度不同 , 看看是否能純化查看更多
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