HRID434569

反应详情

EQUATION

反应方程式

HRID 434569 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-ethyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-quinoline-3-carboxylic acid (0.43 g), 3-hydroxypiperidine (1.6 g), and pyridine (3 ml) was refluxed for 6 hours. The mixture was evaporated to dryness, treated with water, acidified with acetic acid, and extracted with dichloromethane. The dichloromethane layer was washed with water, dried over anhydrous sodium sulfate, and evaporated. The residue was recrystallized from a mixture of DMF and ethanol to give 1-ethyl-6,8-difluoro-1,4-dihydro-7-(3-hydroxy-1-piperidinyl)-4-oxoquinoline-3-carboxylic acid (0.3 g), mp 232°-234° C.

WORKUP

后处理

  1. temperaturewas refluxed for 6 hours
  2. customThe mixture was evaporated to dryness
  3. additiontreated with water
  4. extractionextracted with dichloromethane
  5. washThe dichloromethane layer was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customevaporated
  8. customThe residue was recrystallized from a mixture of DMF and ethanol