HRID1277815

反应详情

EQUATION

反应方程式

HRID 1277815 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

203 mg (1.5 mmol) of phenyl isothiocyanate was added to a solution of 186 mg (1.5 mmol) of 2-methoxy-4-aminopyridine in 15 ml of dry acetone. The mixture was then refluxed for 33 hrs. After cooling, solvent was evaporated off by distillation and the residue was chromatographed in a conventional manner using silica gel (solvent, CHCl3 :acetone=10:1 volume). Fractions were collected and solvent removed by distillation. The residue was recrystallized from ether to give the desired product having a melting point of 138°-141° C. in an amount of 130 mg (yield 33.4%).

WORKUP

后处理

  1. temperatureThe mixture was then refluxed for 33 hrs
  2. temperatureAfter cooling
  3. customsolvent was evaporated off by distillation
  4. customthe residue was chromatographed in a conventional manner
  5. customFractions were collected
  6. customsolvent removed by distillation
  7. customThe residue was recrystallized from ether