反应详情

温度

20 °C

A solution of 1.86 g of 4-(2-pyridylmethyl)piperazine 2,6-dione in 30 ml of dimethylformamide is added at 20° C. to a suspension of 0.36 g of sodium hydride. The mixture is brought to 60° C. for 30 minutes and 2.7 g of 1-(3-chloropropyl)-4-(4-fluorobenzoyl)piperidine, dissolved in 30 ml of dimethylformamide, are then added, again at 20° C. The mixture is kept stirring at 20° C. for approximately 15 hours and the reaction is completed by bringing to 70° C. for 2 hours. After concentration, the residue is taken up in water and the product is extracted with benzene. The oil obtained is purified by chromatography under pressure on 280 g of b 230-400 mesh silica, eluting with a mixture of dichloromethane and methanol (93.5:6.5 V/V). The base obtained is converted to the hydrochloride in ethanol. The precipitate obtained is then filtered off.

1. additionare then added, again at 20° C
2. waitby bringing to 70° C. for 2 hours
3. concentrationAfter concentration
4. extractionthe product is extracted with benzene
5. customThe oil obtained
6. customis purified by chromatography under pressure on 280 g of b 230-400 mesh silica
7. washeluting with a mixture of dichloromethane and methanol (93.5:6.5 V/V)
8. customThe base obtained
9. customThe precipitate obtained
10. filtrationis then filtered off