HRID637290

反应详情

EQUATION

反应方程式

HRID 637290 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

21.2 g of sodium fluoride are added to a solution of 107.8 g of ethyl 2-(2,3,4,5-tetrafluorobenzoyl)-3-cyclopropylamino-acrylate (6) in 400 ml of anhydrous dimethylformamide. Thereafter, the mixture is stirred under reflux for 2 hours, and the hot reaction mixture is poured onto ice. The precipitate is filtered off under suction, washed thoroughly with water and dried over calcium chloride in vacuo at 100° C. 91.2 g of ethyl 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate (7) of melting point 167°-168° C. are obtained.

WORKUP

后处理

  1. temperatureunder reflux for 2 hours
  2. additionthe hot reaction mixture is poured onto ice
  3. filtrationThe precipitate is filtered off under suction
  4. washwashed thoroughly with water
  5. dry with materialdried over calcium chloride in vacuo at 100° C