Sodium Hydroxide → HCID 15296111, compound

Participants

Reaction Steps

The title compound was prepared following the method of Example 1 from 0.6 g (2.78 mole) of 2-difluoromethylfluorene, 1.14 g of 4-picolylchloride hydrochloride, 32 mg benzyltriethylammonium chloride, 4 ml of 50% sodium hydroxide solution, and 25 ml of toluene by reaction at 50° for 6 hrs. The product was chromatographed (silica, CH2Cl2 /MeOH, 10:1) to yield 0.5 g, m.p. >300°; NMR (CDCl3, 200 MHz) δ: 3.43(S,4H), 6.45(d,J=5.7 Hz,4H), 6.74(t,J=56.6 Hz,1H), 7.26-7.70(m.arom.), 8.1(d,J=5.7 Hz,4H). HRMS calculated for C26H20N2F2 : 398.1595 Found: 398.1583.

Provenance & Evidence