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0 °C

A stirred mixture of 20 g of 1,4-dihydro-6,7-dimethoxy-4-oxo-3-quinolinecarbonitrile and 87 ml of phosphorous oxychloride was refluxed for 2 h, cooled, and evaporated free of volatile matter. The residue was stirred at 0° C. with dichloromethane-water as solid sodium carbonate was added until the aqueous layer was pH 8. The organic layer was separated, washed with water, dried and concentrated. Recrystallization from dichloromethane gave a solid, mp 220-223° C.

1. temperaturewas refluxed for 2 h
2. temperaturecooled
3. customevaporated free of volatile matter
4. additionwas added until the aqueous layer
5. customThe organic layer was separated
6. washwashed with water
7. customdried
8. concentrationconcentrated
9. customRecrystallization from dichloromethane
10. customgave a solid, mp 220-223° C.