反应详情

温度

-78 °C

To a solution of 4.76 g (36 mmol) of malonic acid monoethyl ester and 75 ml of THF at -35° C. was added 25 ml (40 mmol) of 1.5N n-butyl lithium solution. The remaining 25 ml (40 mmol) of 1.5N butyllithium solution was added at 0° . After cooling to -78° C., a solution of the 4.8 g of 2-(dimethyl- amino)-3,4,5,6-tetrafluorobenzoyl chloride in 50 ml of THF was added to the dilithio malonate over a 15 minute period. The reaction mixture was stirred for 1.75 hours while the temperature came up to -30° C. The reaction mixture was poured into ice, water, and 50 ml of 1N HCl. The mixture was extracted with ether and the ether extract was washed with H2O, 5% NaHCO3, and HCl. After drying over MgSO4 the ether solution was concentrated to 4.4 g of oil product. NMR spectra indicated the desired product.

1. customcame up to -30° C
2. extractionThe mixture was extracted with ether
3. extractionthe ether extract
4. washwas washed with H2O, 5% NaHCO3, and HCl
5. dry with materialAfter drying over MgSO4 the ether solution
6. concentrationwas concentrated to 4.4 g of oil product