HRID580590

反应详情

EQUATION

反应方程式

HRID 580590 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6,7,8-trifluoro-1-(2-fluoroethyl)-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (0.5 g), anhydrous acetonitrile (5 ml), cis-3-t-butoxycarbonylamino-4-methylpyrrolidine (0.5 g) and DBU (0.27 g) was refluxed for an hour and then concentrated. The resulting residue was dissolved in chloroform and the solution was washed with 10% aqueous citric acid solution. After concentration of the chloroform layer, the resulting precipitate was triturated in water, and collected by filtration and washed with water, methanol and ether successively to give the title compound (0.51 g) as white powder, mp 217°-219° C.

WORKUP

后处理

  1. temperaturewas refluxed for an hour
  2. concentrationconcentrated
  3. dissolutionThe resulting residue was dissolved in chloroform
  4. washthe solution was washed with 10% aqueous citric acid solution
  5. customAfter concentration of the chloroform layer, the resulting precipitate was triturated in water
  6. filtrationcollected by filtration
  7. washwashed with water, methanol and ether successively