HRID2290328
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
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
- temperaturewas heated at 150° C. to 160° C. for 17 hours
- washwashed with water and brine
- dry with materialdried over sodium sulfate, which
- additionwas treated with silical gel
- filtrationfiltered by suction
- customThe filtrate was evaporated to dryness
- customthe resulting residue was crystallized with diisopropyl ether under ice cooling
- filtrationThe resultant crystals were collected by filtration
- washwashed with diisopropyl ether
- customdried