HRID414218

反应详情

EQUATION

反应方程式

HRID 414218 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (200 mg), 3-(2-fluoroethylaminomethyl)pyrrolidine (165 mg) and 1,8-diazabicyclo[5,4,0]-7-undecene (100 mg) in absolute acetonitrile (2 ml) was refluxed for an hour. After cooling, the reaction mixture was concentrated and to the residue was added acetonitrile-ether (1:1, 5 ml). The solution was allowed to stand overnight at 5° C., then the resulting precipitate was collected by filtration and recrystallized from chloroform-methanol-ether to give the title compound (140 mg), mp 134°-138° C.

WORKUP

后处理

  1. temperaturewas refluxed for an hour
  2. temperatureAfter cooling
  3. concentrationthe reaction mixture was concentrated and to the residue
  4. additionwas added acetonitrile-ether (1:1, 5 ml)
  5. filtrationthe resulting precipitate was collected by filtration
  6. customrecrystallized from chloroform-methanol-ether