HRID2413965

反应详情

EQUATION

反应方程式

HRID 2413965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.26 g (0.01 mole) of 8, 9-dichloro-5-methyl-6, 7-dihydro-1,7-dioxo-1H, 5H-benzo[ij]quinolizine-2-carboxylic acid was suspended in 30 ml of methyl cellosolve, 3.43 g (0.03 mole) of N-ethylpiperazine was added thereto, and this mixture was stirred at 100°-110° C. for 2 hours. The resulting reaction solution was evaporated to dryness under reduced pressure. 30 ml of methanol was added to the resulting residue and this mixture was stirred. The insoluble matter was collected by filtration and recrystallized from ethanol to obtain 3.23 g (80.0% yield) of 9-chloro-5-methyl-8-(4-ethyl-1-piperazinyl)-6,7-dihydro-1, 7-dioxo-1H, 5H-benzo[ij]quinolizine-2-carboxylic acid in the form of yellow crystals. These crystals had a melting point of 295°-298° C. (dec.).

WORKUP

后处理

  1. customThe resulting reaction solution
  2. customwas evaporated to dryness under reduced pressure
  3. addition30 ml of methanol was added to the resulting residue
  4. stirringthis mixture was stirred
  5. filtrationThe insoluble matter was collected by filtration
  6. customrecrystallized from ethanol