HRID1084353

反应详情

EQUATION

反应方程式

HRID 1084353 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 15 g of 8-chloro-3-ethoxycarbonyl-7-fluoro-1-methyl-4-oxo-1,4-dihydro-benzo[b][1,8]naphthyridine in 150 cm3 of acetic acid and 150 cm3 of hydrochloric acid as a 17.5% aqueous solution is heated at a temperature close to 100° C., with stirring, for 4 hours. After cooling to a temperature close to 20° C., the product is drained and washed with twice 150 cm3 of ethanol and then twice 100 cm3 of diethyl ether. 12.7 g of 8-chloro-7-fluoro-1-methyl-4-oxo-1,4-dihydro-benzo[b][1,8]naphthyridine-3-carboxylic acid are obtained in the form of a beige solid which sublimes at 400°-405° C. and is used for the subsequent steps without further purification.

WORKUP

后处理

  1. temperatureis heated at a temperature
  2. customclose to 100° C.
  3. temperatureAfter cooling to a temperature
  4. customclose to 20° C.
  5. washwashed with twice 150 cm3 of ethanol