HRID1111448

反应详情

EQUATION

反应方程式

HRID 1111448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid (200 mg), N-methylpiperazine (140 mg) and anhydrous DMSO (3 ml) was stirred for 5 hours at 70° to 95° C. on an oil bath. The reacting mixture was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography eluting with chloroform-methanol-concentrated aqueous ammonia (20:6:1), the residue was recrystallized from methanol to give the title compound (50 mg) as colorless needles, mp 221°-222° C. (decompd.).

WORKUP

后处理

  1. concentrationThe reacting mixture was concentrated under reduced pressure
  2. customThe resulting residue was purified by silica gel column chromatography
  3. washeluting with chloroform-methanol-concentrated aqueous ammonia (20:6:1)
  4. customthe residue was recrystallized from methanol