HRID2290328

反应详情

EQUATION

反应方程式

HRID 2290328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-methyl-3-methylthio-6-phenyl-1,2,4-triazine (2.17 g) and N,N-diethylethylenediamine (2.99 g) was heated at 150° C. to 160° C. for 17 hours. The reaction mixture was dissolved in ethyl acetate, washed with water and brine, and then dried over sodium sulfate, which was treated with silical gel and filtered by suction. The filtrate was evaporated to dryness and the resulting residue was crystallized with diisopropyl ether under ice cooling. The resultant crystals were collected by filtration, washed with diisopropyl ether and dried to give 3-(2-diethylaminoethylamino)-5-methyl-6-phenyl-1,2,4-triazine (1.83 g).

WORKUP

后处理

  1. temperaturewas heated at 150° C. to 160° C. for 17 hours
  2. washwashed with water and brine
  3. dry with materialdried over sodium sulfate, which
  4. additionwas treated with silical gel
  5. filtrationfiltered by suction
  6. customThe filtrate was evaporated to dryness
  7. customthe resulting residue was crystallized with diisopropyl ether under ice cooling
  8. filtrationThe resultant crystals were collected by filtration
  9. washwashed with diisopropyl ether
  10. customdried