HRID224587

反应详情

EQUATION

反应方程式

HRID 224587 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.8 g of the ester of Example 1, 25 ml of N sodium hydroxide solution, 25 ml of water and 100 ml of methanol was heated at 70°-75° C. for 90 minutes and the methanol was then evaporated. 100 ml of water and 10 ml of dimethylformamide were added to the mixture which was then heated to reflux. 4 ml of acetic acid were added thereto and the mixture was held in an ice bath for an hour and was then vacuum filtered. The recovered crystals were washed with water and dried to obtain 1.715 g of 2-(7-chloro-4-quinolinylamino)-5-fluoro-benzoic acid melting at 341°-342° C.

WORKUP

后处理

  1. customthe methanol was then evaporated
  2. addition100 ml of water and 10 ml of dimethylformamide were added to the mixture which
  3. temperaturewas then heated to reflux
  4. addition4 ml of acetic acid were added
  5. waitthe mixture was held in an ice bath for an hour
  6. filtrationvacuum filtered
  7. washThe recovered crystals were washed with water
  8. customdried