反应详情

温度

132.5 °C

A mixture of 86.5 mg (0.25 mmol) of 8-chloro-3-[2-(4-morpholinyl)ethyl]-3H-imidazo[4,5-g]quinoline-7-carbonitrile, 67.2 mg (0.39 mmol) of 4-chloro-5-methoxy-2-methyl aniline and 28.9 mg (0.25 mmol) of pyridine hydrochloride in 3 mL of 2-ethoxyethanol is heated at 130-135° C. for 11 hours. After cooling, the mixture is diluted with water and neutralized with 2 equivalents of sodium carbonate, and then extracted with ethyl acetate. The separated organic layer is washed with brine and dried over sodium sulfate. Removal of the solvent yields a residue which is purified on preparative TLC (developing solvent: 1:9 methanol/methylene chloride), giving 83.3 mg (69.9%) of the product as a beige solid, mp 246-248° C.

1. temperatureAfter cooling
2. extractionextracted with ethyl acetate
3. washThe separated organic layer is washed with brine
4. dry with materialdried over sodium sulfate
5. customRemoval of the solvent
6. customyields a residue which
7. customis purified on preparative TLC (developing solvent: 1:9 methanol/methylene chloride)