HRID1441014

反应详情

EQUATION

反应方程式

HRID 1441014 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirring mixture of 5.0 grams (0.020 mole) of 3,5-diamino-6-(3,4-dichlorophenyl)-1,2,4-triazine (Compound 24; disclosed in J. Med. Chem., 1972, Vol. 15, No 8. 859-861), 2.0 grams (0.020 mole) of acetic anhydride and 0.01 gram (catalyst) of 4-dimethylaminopyridine in 40 mL of dioxane is heated at reflux for about two hours. The mixture is cooled and concentrated under reduced pressure to a residue. The residue is purified by column chromatography on silica gel, yielding 5-amino-3-methylcarbonylamino-6-(3,4-dichlorophenyl)-1,2,4-triazine.

WORKUP

后处理

  1. temperatureat reflux for about two hours
  2. temperatureThe mixture is cooled
  3. concentrationconcentrated under reduced pressure to a residue
  4. customThe residue is purified by column chromatography on silica gel