反应详情

温度

100 °C

To 0.15 g (0.552 mmol) of (8S)-2-chloro-3-fluoro-8-(trifluoromethyl)-6,7,8,9-tetrahydro-4H-pyrimido[1,2-a]pyrimidin-4-one, in solution in 3 cm3 of acetonitrile, are added at a temperature close to 20° C., 0.157 g (0.607 mmol) of 2-isopropoxy-ethyl toluene-4-sulfonate and 0.2 g (0.607 mmol) of cesium carbonate. After 1 hour of stirring at 100° C. in a microwave appliance, the reaction medium is poured into 25 cm3 of ethyl acetate and then washed twice with 10 cm3 of distilled water. The organic phase is dried on anhydrous magnesium sulfate, filtered and dry concentrated under reduced pressure (2.7 kPa) in order to obtain 0.254 g of a residue. This residue is purified by flash chromatography on silica [eluent: cyclohexane/ethyl acetate (8/2 by volume)]. After concentration of the fractions under reduced pressure (2.7 kPa), 0.86 g of (8S)-2-chloro-3-fluoro-9-(2-isopropoxy-ethyl)-8-(trifluoromethyl)-6,7,8,9-tetrahydro-4H-pyrimido[1,2-a]-pyrimidin-4-one are obtained as a colorless oil including the following characteristics:

1. customclose to 20° C.
2. washwashed twice with 10 cm3 of distilled water
3. dry with materialThe organic phase is dried on anhydrous magnesium sulfate
4. filtrationfiltered
5. customdry
6. concentrationconcentrated under reduced pressure (2.7 kPa) in order