反应详情

The title compound was prepared following the procedure of Example 1 from 0.43 g (2.56 mmole) of 4,5-diazafluorene, 0.84 g of 4-picolylchloride hydrochloride, 29.0 mg of benzyltriethylammonium chloride, 3 ml of 50% sodium hydroxide, and 30 ml toluene by reaction at 50° for 6 hrs. The crude product was chromatographed (Ethylacetate/Methanol, 99:1) and recrystallized from isopropyl alcohol. NMR (CDCl3,200 MHz) δ: 3.42(s,4H), 6.52(d,J=5.7 Hz,4H), 7.33(dd,2H), 7.85(d,2H), 8.16(d,J=5.6 Hz,4H), 8.61(d,2H).

1. customby reaction at 50° for 6 hrs
2. customThe crude product was chromatographed (Ethylacetate/Methanol, 99:1)
3. customrecrystallized from isopropyl alcohol