HRID1607084

反应详情

EQUATION

反应方程式

HRID 1607084 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.3 g (76 mmol) of 6-amino-2-hydroxypyridine and 20 g (114 mmol) of N,N-di-n-propylformamide dimethyl acetal are placed in 70 ml of xylene under argon. .The whole is heated at 100° for 1/2 hour while stirring It is then allowed to cool, is concentrated by evaporation under a water-jet vacuum and the residue is filtered over 10 times the amount of Florisil using methylene chloride. The fractions containing the product are concentrated by evaporation and then crystallised from n-hexane. N-(2-hydroxy-6-pyridyl)-N',N'-di-n-propylformamidine and N-(2-pyridon-6-yl)-N',N'-di-n-propylformamidine having a melting point of 102°-104° are obtained.

WORKUP

后处理

  1. temperature.The whole is heated at 100° for 1/2 hour
  2. temperatureto cool
  3. concentrationis concentrated by evaporation under a water-jet vacuum
  4. filtrationthe residue is filtered over 10 times the amount of Florisil
  5. additionThe fractions containing the product
  6. concentrationare concentrated by evaporation
  7. customcrystallised from n-hexane