反应详情

温度

75 °C

A suspension of ethyl 3-(2-chloro-6,7,8-trifluoro-3-quinolyl)-3-oxopropionate (26.7 g) in ethyl acetate (270 cc) and N,N-dimethylformamide dimethyl acetal (32 cc) is heated to a temperature in the region of 75° C. with stirring for 2 hours. The reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. The dry extract is taken up with isopropyl ether (175 cc), drained and washed with the same solvent (2×85 cc). Ethyl 2-(2-chloro-6,7,8-trifluoro-3-quinolinecarbonyl)-3-(dimethylamino)acrylate (19.32 g) is obtained in the form of an orange-colored solid, m.p. 118° C., which is used without further purification for the subsequent steps.

1. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C
2. extractionThe dry extract
3. washwashed with the same solvent (2×85 cc)