HRID1196840

反应详情

EQUATION

反应方程式

HRID 1196840 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 1-cyclopropyl-8-ethenyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (0.80 g, 2.9 mmol), 2-methylpiperazine (1.9 g, 19 mmol) and acetonitrile (5 mL) was heated at reflux for 22 hours. The mixture was cooled and concentrated. The residue was dissolved in H2O (50 mL), treated with charcoal and filtered through celite. The pH of the filtrate was adjusted to 7, with HCl (3N) and after cooling to 0° C. the precipitate was collected and dried to provide 0.81 g (78%) of the desired product; mp 227°-231° dec.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 22 hours
  3. temperatureThe mixture was cooled
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in H2O (50 mL)
  6. additiontreated with charcoal
  7. filtrationfiltered through celite
  8. customwas collected
  9. customdried