反应详情

温度

120 °C

Put 72 g (227.6 mmol) 5-(4-ethylphenyl)-6-phenylfuro[2,3-d]pyrimidin-4(3H)-one in 360 ml (4.6 mol) phosphoryl chloride and heat to reflux. Stir the mixture for approx. 1 h at 120° C., before adding the reaction mixture dropwise, after cooling to RT, at controlled dose and with vigorous stirring, to a mixture of 2.2 litres of 25% ammonia solution and 1.2 litres water (pH>9, temperature 55-75° C.). Extract the aqueous mixture three times with dichloromethane, combine the organic phases, dry over sodium sulphate and concentrate by vacuum evaporation. Wash the residue with a little diisopropyl ether, and after filtration and drying at high vacuum, 66.1 g (85.2% of theor.) of the target product is obtained.

1. additionbefore adding the reaction mixture dropwise
2. extractionExtract the aqueous mixture three times with dichloromethane
3. dry with materialdry over sodium sulphate
4. concentrationconcentrate by vacuum evaporation
5. washWash the residue with a little diisopropyl ether
6. filtrationafter filtration
7. customdrying at high vacuum, 66.1 g (85.2% of theor.) of the target product
8. customis obtained