HRID413060

反应详情

EQUATION

反应方程式

HRID 413060 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A suspension of 0.70 g of ethyl 9-fluoro-8-[4-(4-fluorophenyl)piperazin-1-yl]-4-methyl-1-oxo-1,4-dihydrobenzo[f][1,7]naphthyridine-2-carboxylate in a mixture of 250 cm3 of ethanol at 40% and 4 cm3 of a 1 N aqueous potassium hydroxide solution was heated, with stirring, for 8 hours at a temperature of 80° C. After cooling to a temperature of 60° C., the light insoluble material was removed by filtration. The solution was neutralized with 4.1 cm3 of a 1 N aqueous hydrochloric acid solution; the insoluble material formed was dewatered, washed 3 times with 20 cm3 of water and twice with 20 cm3 of ethanol and dried under vacuum at 100° C. 0.56 g of 9-fluoro-8-[4-(4-fluorophenyl)piperazin-1-yl]-4-methyl-1-oxo-1,4-dihydrobenzo[f][1,7]naphthyridine-2-carboxylic acid was obtained in the form of yellow crystals, which melted at 346° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureAfter cooling to a temperature of 60° C.
  3. customthe light insoluble material was removed by filtration
  4. customthe insoluble material formed
  5. washwashed 3 times with 20 cm3 of water
  6. dry with materialtwice with 20 cm3 of ethanol and dried under vacuum at 100° C