反应详情

A suspension of 16.5 g of ethyl 3-(2,7-dichloro-6-fluoro-3-quinolyl)-3-oxopropionate in 160 cm3 of ethyl acetate and 19 cm3 of N,N-dimethylformamide dimethyl acetal is heated at a temperature close to 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 in 50 cm3 of diisopropyl ether, drained and washed with twice 10 cm3 of diisopropyl ether. 16.57 g of ethyl 2-(2,7-dichloro-6-fluoro-quinoline-3-carbonyl)-3-dimethylaminoacrylate are obtained in the form of an orange solid melting at 122° C. This product is used for the subsequent steps without further purification.

1. temperatureis heated at a temperature
2. customclose to 75° C.
3. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (20 kPa) at 50° C
4. extractionThe dry extract
5. washwashed with twice 10 cm3 of diisopropyl ether