HRID544221

反应详情

EQUATION

反应方程式

HRID 544221 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-7-chloro-1,4-dihydro-6-fluoro-4-oxoquinoline-3-carboxylic acid (0.80 g), 2-oxopiperazine (3.0 g) and 4 ml pyridine was heated for 18 hours. The reaction mixture was evaporated under vacuum, an aqueous solution of caustic soda was added to adjust the pH to 10, ice cooled and the undissolved matter was collected and washed with a small amount of an aqueous solution of NaOH. The filtered product was suspended in water, acidified with acetic acid, filtered and washed. The product obtained was dissolved in an aqueous solution of NaOH and acidified with acetic acid. The precipitate was filtered, washed and dried to obtain 0.32 g (32%) of 1-ethyl-1,4-dihydro-6-fluoro-7-(3-oxo-1-piperazinyl)-4-oxoquinoline-3-carboxylic acid.

WORKUP

后处理

  1. temperaturewas heated for 18 hours
  2. customThe reaction mixture was evaporated under vacuum
  3. additionan aqueous solution of caustic soda was added
  4. temperaturecooled
  5. customthe undissolved matter was collected
  6. washwashed with a small amount of an aqueous solution of NaOH
  7. filtrationfiltered
  8. washwashed
  9. customThe product obtained
  10. filtrationThe precipitate was filtered
  11. washwashed
  12. customdried