HRID1277812

反应详情

EQUATION

反应方程式

HRID 1277812 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

112 mg (1 mmol) of 2-fluoro-4-aminopyridine was added to 9 ml of dry benzene and to the resulting solution was further added 119 mg (1 mmol) of phenyl isocyanate. After stirring at room temperature for 30 hrs., the crystals which deposited were collected by filtration and then subjected to chromatography in a conventional manner using alumina. After developing the column with a benzene-ethyl acetate (3:1 by volume) solvent mixture, eluate containing the objective compound was collected. After distilling solvent off under reduced pressure, the residue was recrystallized from an ethyl acetate-n-hexane solvent mixture to give 113 mg of the objective compound: yield 48.9%; m.p. 179°-180° C.

WORKUP

后处理

  1. filtration, the crystals which deposited were collected by filtration
  2. additioneluate containing the objective compound
  3. customwas collected
  4. distillationAfter distilling solvent off under reduced pressure
  5. customthe residue was recrystallized from an ethyl acetate-n-hexane solvent mixture