反应详情

POCl3 (15 ml) was added to 6-chloro-2-oxo-4-phenyl-1,2-dihydro-quinoline-3-carboxylic acid ethyl ester (3 g, 9.15 mmol) and refluxed for 1 h. Then the reaction mixture was cooled to room temperature and diluted with cold water and the pH was adjusted to 7 with ammonia solution and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, concentrated in vacuo to afford a crude residue which was purified by flash column chromatography (100-200 mesh silica, eluting with 5-10% ethyl acetate in hexane) to afford pure 2,6-dichloro-4-phenyl-quinoline-3-carboxylic acid ethyl ester (2 g, 63%) as pale yellow solid. LC-MS: 346 (M+H)+.

1. temperaturerefluxed for 1 h
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customto afford a crude residue which
7. customwas purified by flash column chromatography (100-200 mesh silica, eluting with 5-10% ethyl acetate in hexane)