反应详情

A mixture of 252.6 mg (0.6 mmol) of 4-(2,4-dichloroanilino)-7,8-dimethoxybenzo[g]quinoline-3-carbonitrile and 5.0 g of pyridine hydrochloride is heated at 215–220° C. for 40 minutes under nitrogen. After cooling, the mixture is neutralized with 3% ammonium hydroxide aqueous solution and stirred for 30 minutes. The precipitate is collected, washed with water and dried in vacuo. The crude product is passed through a short column of silica gel, eluting with a gradient of methylene chloride/methanol 90:10 to 50:50, to provide 122.8 mg (51.7%) of the product as a brown solid, mp>260° C.

1. temperatureis heated at 215–220° C. for 40 minutes under nitrogen
2. temperatureAfter cooling
3. customThe precipitate is collected
4. washwashed with water
5. customdried in vacuo
6. washeluting with a gradient of methylene chloride/methanol 90:10 to 50:50