HRID248462

反应详情

EQUATION

反应方程式

HRID 248462 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 1.7 g portion of 2-(methoxymethyl)piperazine was dissolved in 8 ml of pyridine. A 0.88 g portion of 7-chloro-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid was added and the mixture was heated in a pressure bottle, under argon, at 120°-130° C. for 18 hours. The solvents were removed and the resulting gum evaporated three times from toluene. The residue was purified by column chromatography, eluting with chloroform:methanol saturated with water (90:10). The appropriate fractions were combined and evaporated, giving 550 mg of the desired product, mp 169°-170° C.

WORKUP

后处理

  1. temperaturethe mixture was heated in a pressure bottle, under argon, at 120°-130° C. for 18 hours
  2. customThe solvents were removed
  3. customthe resulting gum evaporated three times from toluene
  4. customThe residue was purified by column chromatography
  5. washeluting with chloroform
  6. customevaporated