HRID1094217

反应详情

EQUATION

反应方程式

HRID 1094217 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

15 ml of methanol, 15 ml of THF and 250 mg of sodium cyanoborohydride were added to 300 mg of 7-(cyclohexylamino)-1-cyclopentyl-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carbaldehyde oxime. 2 ml of a 4 M hydrogen chloride dioxane solution was added thereto under ice-cooling, followed by stirring at room temperature for 3 hours. Under ice-cooling, aqueous 1 M sodium hydroxide solution was added thereto, followed by extraction with chloroform and subsequent washing with aqueous saturated sodium chloride. After drying over anhydrous sodium sulfate, the solvent was evaporated under a reduced pressure, and the resulting residue was purified by silica gel column chromatography to obtain 130 mg of 7-(cyclohexylamino)-1-cyclopentyl-6-fluoro-3-[(hydroxyamino)methyl]quinolin-4(1H)-one.

WORKUP

后处理

  1. temperatureunder ice-cooling
  2. temperatureUnder ice-cooling
  3. extractionfollowed by extraction with chloroform
  4. washsubsequent washing with aqueous saturated sodium chloride
  5. dry with materialAfter drying over anhydrous sodium sulfate
  6. customthe solvent was evaporated under a reduced pressure
  7. customthe resulting residue was purified by silica gel column chromatography