反应详情

2.6 g of ethyl 2-(2-methyl-3,4,6-trifluorobenzoyl)-3-cyclopropylaminoacrylate was dissolved in 26 ml of anhydrous dioxane, and thereto 0.38 g of 60% sodium hydride was added portionwise under ice-cooling. After stirring at room temperature for 30 minutes, the mixture was poured into ice water and extracted with dichloromethane. The extract was dried over magnesium sulfate and concentrated. Diethyl ether was added to the residue and the resulting crystals were filtered, followed by recrystallization from ethanol to give 2.0 g of ethyl 1-cyclopropyl-6,7-difluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylate.

1. temperaturecooling
2. extractionextracted with dichloromethane
3. dry with materialThe extract was dried over magnesium sulfate
4. concentrationconcentrated
5. additionDiethyl ether was added to the residue
6. filtrationthe resulting crystals were filtered
7. customfollowed by recrystallization from ethanol