HRID1277815
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was then refluxed for 33 hrs
- temperatureAfter cooling
- customsolvent was evaporated off by distillation
- customthe residue was chromatographed in a conventional manner
- customFractions were collected
- customsolvent removed by distillation
- customThe residue was recrystallized from ether