HRID580572

反应详情

EQUATION

反应方程式

HRID 580572 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (0.5 g), anhydrous acetonitrile (5 ml), 3-t-butoxycarbonylamino-4-methylpyrrolidine (0.5 g) and DBU (0.25 g) was refluxed for an hour. The reacting mixture was concentrated under reduced pressure, to the resulting residue was added acetonitrile-ether (1:1) to crystallize and the precipitate was collected by filtration. This precipitate was recrystallized from dichloromethane-methanol to give the title compound (0.4 g) as pale yellow powder, mp 213°-215° C.

WORKUP

后处理

  1. temperaturewas refluxed for an hour
  2. concentrationThe reacting mixture was concentrated under reduced pressure, to the resulting residue
  3. additionwas added acetonitrile-ether (1:1)
  4. customto crystallize
  5. filtrationthe precipitate was collected by filtration
  6. customThis precipitate was recrystallized from dichloromethane-methanol