反应详情

温度

20 °C

4 g of caesium carbonate and 796 mg of benzyl bromide are added to a suspension of 1 g of (8S)-3-fluoro-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetrahydro-4 H-pyrimido[1,2-a]pyrimidin-4-one in 11.8 ml of acetonitrile. After stirring overnight at a temperature in the region of 20° C., the suspension obtained is filtered and the resulting filtrate is concentrated to dryness under reduced pressure. The oily yellow residue is purified on a silica column (eluent: CH2Cl2/MeOH 98/02). The fractions of interest are combined and concentrated to dryness under reduced pressure. The residue is taken up with diethyl ether, spin-filter-dried and then dried under vacuum. 600 mg of (8S)-9-benzyl-3-fluoro-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetra-hydro-4 H-pyrimido[1,2-a]pyrimidin-4-one are thus obtained in the form of a white powder, the characteristics of which are the following:

1. customthe suspension obtained
2. filtrationis filtered
3. concentrationthe resulting filtrate is concentrated to dryness under reduced pressure
4. customThe oily yellow residue is purified on a silica column (eluent: CH2Cl2/MeOH 98/02)
5. concentrationconcentrated to dryness under reduced pressure
6. customspin-filter-dried
7. customdried under vacuum