反应详情

A mixture of 3-ethoxycarbonyl-8-nitro-4-oxo-3,4-dihydro-quinoline (10.2 g) and phosphorous oxychloride (10 ml) was stirred at reflux for 2 hours. The warm reaction mixture was added cautiously to a vigorously stirred mixture of ice, concentrated aqueous ammonia and chloroform. The organic layer was separated, washed with water, dried and evaporated to dryness. The residue was purified by flash chromatography on silica using chloroform as eluant to give 4-chloro-3-ethoxycarbonyl-8-nitro-quinoline in 75% yield, mp 253-254° C.

1. temperatureat reflux for 2 hours
2. customThe warm reaction mixture
3. customThe organic layer was separated
4. washwashed with water
5. customdried
6. customevaporated to dryness
7. customThe residue was purified by flash chromatography on silica