反应详情

温度

75 °C

A suspension of ethyl 3-(2,7-dichloro-6-fluoro-3-quinolinyl)-3-oxopropionate (16.5 g) in ethyl acetate (160 cc) and N,N-dimethylformamide dimethyl acetal (19 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 50° C. The dry extract is taken up with isopropyl ether (50 cc), drained and washed with isopropyl ether (2×10 cc). Ethyl 2-(2,7-dichloro-6-fluoro-3-quinolinecarbonyl)-3-(dimethylamino)acrylate (16.57 g) is obtained in the form of an orange-colored solid, m.p. 122° C. This product is used without further purification for the subsequent steps.

1. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at 50° C
2. extractionThe dry extract
3. washwashed with isopropyl ether (2×10 cc)