反应详情

温度

120 °C

A mixture of 1-(4-chlorobutyl)-3-methoxy-1H-pyridin-2-one (0.93 mmol, 0.20 g) from Example 5.1, 2-tert-butyl-4-piperazin-1-yl-6-propylpyrimidine (0.93 mmol, 0.24 g; prepared as described in DE 19735410), sodium bromide (4.64 mmol, 0.48 g), ethyldiisopropylamine (9.09 mmol, 1.17 g) and N-methylpyrrolidinone (0.5 ml) was heated at 120° C. for 6 hours. The resulting suspension was filtered with suction and the filtrate was concentrated. The residue obtained in this way was taken up in ethyl acetate/water. The aqueous mixture was adjusted to pH 5.5 with sodium bicarbonate and the aqueous mixture was extracted several times with diethyl ether. The organic phase was then dried, the desiccant was removed by filtration, and the organic phase was concentrated under reduced pressure. Chromatography of the residue on silica gel (eluent: CH2Cl2/CH3OH (0-2%) afforded 0.24 g of the title compound.

1. filtrationThe resulting suspension was filtered with suction
2. concentrationthe filtrate was concentrated
3. customThe residue obtained in this way
4. extractionthe aqueous mixture was extracted several times with diethyl ether
5. customThe organic phase was then dried
6. customthe desiccant was removed by filtration
7. concentrationthe organic phase was concentrated under reduced pressure