反应详情

温度

150 °C

To a stirred solution of 2,6-dichloro-4-phenyl-quinoline-3-carboxylic acid ethyl ester (prepared as described in example 11 step B, 100 mg, 0.29 mmol) in a sealed tube was added morpholine (0.038 ml, 0.43 mmol). Then the mixture was stirred at 150° C. for 3 h. After cooling, this reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and concentrated in vacuo to afford a crude residue which was purified by flash column chromatography (100-200 mesh silica, eluting with 10% ethyl acetate in hexane) to give 6-chloro-2-morpholin-4-yl-4-phenyl-quinoline-3-carboxylic acid ethyl ester (65 mg, 57%) as pale yellow solid. LC-MS: 397 (M+H)+.

1. temperatureAfter cooling
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 10% ethyl acetate in hexane)