HRID1461384

反应详情

EQUATION

反应方程式

HRID 1461384 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

Potassium carbonate (30 g) was added to a stirred solution/suspension of 31.65 g ethyl 2-(4-bromo-2,3,5,6-tetrafluorobenzoyl)-3-cyclopropylaminopropenoate in 300 ml dimethylformamide. The mixture was heated at 150° C. for 1.5 hours, then cooled, poured into water and extracted with methylene dichloride. The extract was washed with water and sodium chloride solution, dried (magnesium sulfate) and concentrated. The residue was recrystallized from acetonitrile to give 19.3 g (64%) ethyl 7-bromo-1-cyclopropyl-5,6,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate, m.p. 187°-189° C.

WORKUP

后处理

  1. temperaturecooled
  2. extractionextracted with methylene dichloride
  3. washThe extract was washed with water and sodium chloride solution
  4. dry with materialdried (magnesium sulfate)
  5. concentrationconcentrated
  6. customThe residue was recrystallized from acetonitrile