HRID1463672

反应详情

EQUATION

反应方程式

HRID 1463672 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The title compound was prepared following the method of Example 1 from 4.0 g (21.74 mmole) of 2-fluorofluorene, 8.92 g of 4-picolylchloride hydrochloride, 120 ml of toluene, 200 mg of benzyltriethylammonium chloride, and 20 ml of 50% sodium hydroxide by reaction at 22° for 17 hrs. The product was chromatographed (silica, CH2Cl2 /MeOH, 10:1) to yield 2.9 g which was recrystallized (ethanol-acetone) and converted to the dihydrochloride, m.p. >300°.

WORKUP

后处理

  1. customby reaction at 22° for 17 hrs
  2. customThe product was chromatographed (silica, CH2Cl2 /MeOH, 10:1)
  3. customto yield 2.9 g which
  4. customwas recrystallized (ethanol-acetone)