HRID236678

反应详情

EQUATION

反应方程式

HRID 236678 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture containing 8.2 g. of 4-chloro-6-methyl-2-(4-pyridinyl)pyrimidine, 8.7 g. of diethylamine hydrochloride, 100 ml. of ethanol, 6 g. of potassium carbonate and 10 ml. of water was refluxed with stirring for eight hours and then concentrated in vacuo to dryness. The residue was swirled in water and the solid collected. The solid was dissolved in boiling isopropyl alcohol, the hot solution treated with decolorizing charcoal and filtered, and the hot filtrate allowed to cool. The filtrate was then saturated with gaseous hydrogen chloride, ether was added to turbidity and the mixture was allowed to stand. The separated solid was collected and dried in vacuo at 80° C. to yield 7.4 g. of N,N-diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine dihydrochloride, m.p. 205°-208° C.

WORKUP

后处理

  1. additionA mixture containing 8.2 g
  2. concentrationconcentrated in vacuo to dryness
  3. customthe solid collected
  4. dissolutionThe solid was dissolved
  5. additionthe hot solution treated with decolorizing charcoal
  6. filtrationfiltered
  7. temperatureto cool
  8. additionsaturated with gaseous hydrogen chloride, ether was added to turbidity
  9. customThe separated solid was collected
  10. customdried in vacuo at 80° C.
  11. customto yield 7.4 g