反应详情

To methylene chloride (120 ml) solution of methyl 3-dimethylamino -2-(2,3,4,5-tetrafluorobenzoyl)acrylate (13.2 g) was added methylene chloride (12 ml) solution of 1-tert-butoxycarbonyl-1-methylhydrazine (7.59 g) with ice-cooling, and the mixture was stirred for one hour at the same temperature and then for 15 hours at room temperature. The reaction mixture was concentrated under reduced pressure. The residue was triturated with diisopropyl ether (132 ml). The solid formed was taken out by filtration and dried with phosphorus pentaoxide under reduced pressure to obtain methyl 1-(N-tert-butoxycarbonyl-N-methylamino)-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylate (10.49 g).

1. temperaturecooling
2. waitfor 15 hours at room temperature
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. customThe residue was triturated with diisopropyl ether (132 ml)
5. customThe solid formed
6. filtrationwas taken out by filtration
7. dry with materialdried with phosphorus pentaoxide under reduced pressure