HRID1066767

反应详情

EQUATION

反应方程式

HRID 1066767 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,5-Dinitro-1-methyl-2-pyridone (5.97 g; 30 mmol) was treated with 1.22M ammonia in methanol (300 ml) then 1-methyl-4-piperidone (3.73 g, 33 mmol) and the mixture heated at 60° for 5 h, then allowed to stand at ambient temp for 72 h. Evaporation in vacuo gave an orange/red residue which was triturated in dichloromethane and diethyl ether, collected by filtration, washed with diethyl ether and dried in air. Chromatography through silica gel, eluting with ethyl acetate, gave the title compound as a red solid (3.4 g, 59%).

WORKUP

后处理

  1. customEvaporation in vacuo
  2. customgave an orange/red residue which
  3. customwas triturated in dichloromethane
  4. filtrationdiethyl ether, collected by filtration
  5. washwashed with diethyl ether
  6. customdried in air
  7. washChromatography through silica gel, eluting with ethyl acetate