反应详情

1.8 g (8.4 mmol) of 1-cyclobutylpiperazine dihydrochloride (Zaragoza et al., J. Med. Chem. 2004, 47, 2833) are initially charged in 18 ml of water, and 2.9 ml (2.1 g, 16.9 mmol) of N-ethyl-N-(propan-2-yl)propane-2-amine are added. The mixture is stirred at RT for 30 min, and 1.3 g (8.4 mmol) of 4,6-dichloropyrimidine are added. The reaction mixture is stirred at 115° C. for 1 h and cooled to RT, 25 ml of ethyl acetate are added and the mixture is extracted with 25 ml of a saturated aqueous sodium bicarbonate solution. The organic phase is separated off, dried over sodium sulphate, filtered and concentrated under reduced pressure. The crude product is purified by column chromatography on silica gel (mobile phase: dichloromethane/methanol 100/3). Yield: 1.9 g (89% of theory)

1. stirringThe reaction mixture is stirred at 115° C. for 1 h
2. temperaturecooled to RT
3. extractionthe mixture is extracted with 25 ml of a saturated aqueous sodium bicarbonate solution
4. customThe organic phase is separated off
5. dry with materialdried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe crude product is purified by column chromatography on silica gel (mobile phase: dichloromethane/methanol 100/3)